Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Jian-Fang Ma' _publ_contact_author_address ; Department of Chemistry Northeast Normal University No. 5268, Renmin Street Changchun 130024 CHINA ; _publ_contact_author_email JIANFANGMA@YAHOO.COM.CN _publ_section_title ; Syntheses, structures and luminescent properties of zinc(II) and cadmium(II) coordination complexes based on bis(imidazole) and different carboxylate ligands ; loop_ _publ_author_name 'Jian-Fang Ma' 'Shun-Li Li' 'Ying-Ying Liu' 'Guo-Hua Wei' 'Jin Yang' ; Lai-Ping Zhang ; data_compound1 _database_code_depnum_ccdc_archive 'CCDC 665624' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H28 N4 O5 Zn' _chemical_formula_sum 'C28 H28 N4 O5 Zn' _chemical_formula_weight 565.91 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.7260(5) _cell_length_b 23.1830(10) _cell_length_c 12.7760(10) _cell_angle_alpha 90.00 _cell_angle_beta 105.5190(10) _cell_angle_gamma 90.00 _cell_volume 2775.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3877 _cell_measurement_theta_min 1.9 _cell_measurement_theta_max 28.3 _exptl_crystal_description Block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.354 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1176 _exptl_absorpt_coefficient_mu 0.928 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.89 _exptl_absorpt_correction_T_max 0.95 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area-detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17051 _diffrn_reflns_av_R_equivalents 0.0454 _diffrn_reflns_av_sigmaI/netI 0.0578 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 28.33 _reflns_number_total 6643 _reflns_number_gt 3877 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0380P)^2^+0.0525P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6643 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0931 _refine_ls_R_factor_gt 0.0420 _refine_ls_wR_factor_ref 0.0974 _refine_ls_wR_factor_gt 0.0819 _refine_ls_goodness_of_fit_ref 0.998 _refine_ls_restrained_S_all 0.998 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.48184(3) 0.055962(12) 0.77100(2) 0.05226(11) Uani 1 1 d . . . C1 C 0.7475(2) 0.03194(10) 0.7021(2) 0.0527(6) Uani 1 1 d . . . H1 H 0.6958 0.0255 0.6305 0.063 Uiso 1 1 calc R . . C2 C 0.8034(3) 0.05202(13) 0.8715(2) 0.0711(8) Uani 1 1 d . . . H2 H 0.7957 0.0622 0.9401 0.085 Uiso 1 1 calc R . . C3 C 0.9261(3) 0.04077(12) 0.8461(2) 0.0665(7) Uani 1 1 d . . . H3 H 1.0175 0.0416 0.8930 0.080 Uiso 1 1 calc R . . C4 C 0.9880(3) 0.01484(13) 0.6726(2) 0.0745(8) Uani 1 1 d . . . H4A H 0.9486 -0.0162 0.6227 0.089 Uiso 1 1 calc R . . H4B H 1.0780 0.0017 0.7197 0.089 Uiso 1 1 calc R . . C5 C 1.0144(3) 0.06555(13) 0.6095(2) 0.0750(9) Uani 1 1 d . . . H5A H 1.0500 0.0977 0.6579 0.090 Uiso 1 1 calc R . . H5B H 1.0849 0.0561 0.5709 0.090 Uiso 1 1 calc R . . C6 C 0.8802(3) 0.13533(13) 0.4882(2) 0.0832(9) Uani 1 1 d . . . H6A H 0.9455 0.1368 0.4426 0.100 Uiso 1 1 calc R . . H6B H 0.9084 0.1644 0.5444 0.100 Uiso 1 1 calc R . . C7 C 0.7304(3) 0.14592(11) 0.4215(2) 0.0800(9) Uani 1 1 d . . . H7A H 0.6661 0.1439 0.4678 0.096 Uiso 1 1 calc R . . H7B H 0.7236 0.1843 0.3905 0.096 Uiso 1 1 calc R . . C8 C 0.7274(3) 0.10151(11) 0.2394(2) 0.0609(7) Uani 1 1 d . . . H8 H 0.7797 0.1293 0.2142 0.073 Uiso 1 1 calc R . . C9 C 0.6769(3) 0.05195(11) 0.1901(2) 0.0562(6) Uani 1 1 d . . . H9 H 0.6876 0.0397 0.1234 0.067 Uiso 1 1 calc R . . C10 C 0.6157(3) 0.05470(11) 0.3390(2) 0.0561(6) Uani 1 1 d . . . H10 H 0.5770 0.0450 0.3958 0.067 Uiso 1 1 calc R . . C11 C 0.3798(3) 0.09953(11) 0.9401(2) 0.0572(7) Uani 1 1 d . . . C12 C 0.3872(3) 0.14337(11) 1.0263(2) 0.0594(7) Uani 1 1 d . . . H12 H 0.3132 0.1445 1.0597 0.071 Uiso 1 1 calc R . . C13 C 0.4914(2) 0.18049(11) 1.05806(19) 0.0527(6) Uani 1 1 d . . . H13 H 0.5626 0.1786 1.0220 0.063 Uiso 1 1 calc R . . C14 C 0.5107(2) 0.22462(10) 1.1431(2) 0.0516(6) Uani 1 1 d . . . C15 C 0.4070(3) 0.23914(13) 1.1941(3) 0.0839(10) Uani 1 1 d . . . H15 H 0.3186 0.2210 1.1737 0.101 Uiso 1 1 calc R . . C16 C 0.4332(4) 0.28039(15) 1.2751(3) 0.1051(13) Uani 1 1 d . . . H16 H 0.3623 0.2898 1.3087 0.126 Uiso 1 1 calc R . . C17 C 0.5628(3) 0.30756(13) 1.3062(3) 0.0827(9) Uani 1 1 d . . . H17 H 0.5806 0.3346 1.3619 0.099 Uiso 1 1 calc R . . C18 C 0.6648(3) 0.29493(11) 1.2558(2) 0.0689(8) Uani 1 1 d . . . H18 H 0.7522 0.3139 1.2757 0.083 Uiso 1 1 calc R . . C19 C 0.6396(3) 0.25418(11) 1.1756(2) 0.0578(6) Uani 1 1 d . . . H19 H 0.7108 0.2460 1.1416 0.069 Uiso 1 1 calc R . . C20 C 0.3756(3) 0.09828(11) 0.5631(2) 0.0530(6) Uani 1 1 d . . . C21 C 0.2803(3) 0.13629(11) 0.4804(2) 0.0581(7) Uani 1 1 d . . . H21 H 0.2446 0.1695 0.5043 0.070 Uiso 1 1 calc R . . C22 C 0.2446(3) 0.12544(11) 0.3769(2) 0.0580(7) Uani 1 1 d . . . H22 H 0.2845 0.0925 0.3557 0.070 Uiso 1 1 calc R . . C23 C 0.1488(3) 0.15881(12) 0.2888(2) 0.0577(7) Uani 1 1 d . . . C24 C 0.1042(3) 0.13424(14) 0.1866(2) 0.0741(8) Uani 1 1 d . . . H24 H 0.1307 0.0966 0.1763 0.089 Uiso 1 1 calc R . . C25 C 0.0217(3) 0.16455(19) 0.1002(3) 0.0922(11) Uani 1 1 d . . . H25 H -0.0081 0.1472 0.0322 0.111 Uiso 1 1 calc R . . C26 C -0.0163(3) 0.2194(2) 0.1137(3) 0.1055(13) Uani 1 1 d . . . H26 H -0.0695 0.2400 0.0542 0.127 Uiso 1 1 calc R . . C27 C 0.0224(3) 0.24519(16) 0.2139(3) 0.0928(11) Uani 1 1 d . . . H27 H -0.0057 0.2828 0.2226 0.111 Uiso 1 1 calc R . . C28 C 0.1048(3) 0.21428(13) 0.3030(3) 0.0712(8) Uani 1 1 d . . . H28 H 0.1299 0.2311 0.3716 0.085 Uiso 1 1 calc R . . N1 N 0.69049(19) 0.04616(9) 0.78023(16) 0.0541(5) Uani 1 1 d . . . N2 N 0.89016(19) 0.02784(9) 0.73823(17) 0.0534(5) Uani 1 1 d . . . N3 N 0.6872(2) 0.10352(9) 0.33433(17) 0.0568(5) Uani 1 1 d . . . N4 N 0.60692(19) 0.02209(8) 0.25310(16) 0.0518(5) Uani 1 1 d . . . O1 O 0.38307(18) 0.11134(7) 0.66111(15) 0.0635(5) Uani 1 1 d . . . O2 O 0.4389(2) 0.05749(8) 0.53521(15) 0.0748(5) Uani 1 1 d . . . O3 O 0.49185(18) 0.09522(8) 0.90611(14) 0.0692(5) Uani 1 1 d . . . O4 O 0.2710(2) 0.07129(8) 0.90529(17) 0.0818(6) Uani 1 1 d . . . O5 O 0.88326(19) 0.08039(8) 0.53506(15) 0.0706(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.04053(15) 0.0655(2) 0.05243(19) -0.00916(14) 0.01536(12) -0.00284(14) C1 0.0405(12) 0.0647(16) 0.0518(16) 0.0009(12) 0.0105(12) 0.0026(12) C2 0.0545(15) 0.110(2) 0.0501(17) -0.0165(15) 0.0164(13) -0.0158(16) C3 0.0425(13) 0.097(2) 0.0552(18) -0.0005(15) 0.0046(13) -0.0065(14) C4 0.0480(14) 0.102(2) 0.077(2) -0.0017(18) 0.0234(15) 0.0162(15) C5 0.0491(15) 0.115(3) 0.0640(19) -0.0125(17) 0.0206(14) -0.0222(16) C6 0.099(2) 0.077(2) 0.071(2) -0.0097(17) 0.0193(18) -0.0413(18) C7 0.108(3) 0.0496(17) 0.083(2) -0.0074(15) 0.028(2) -0.0065(16) C8 0.0618(16) 0.0595(17) 0.0643(18) 0.0216(14) 0.0218(14) 0.0061(14) C9 0.0567(15) 0.0647(17) 0.0478(15) 0.0087(13) 0.0148(12) 0.0057(13) C10 0.0529(14) 0.0610(16) 0.0566(17) 0.0011(14) 0.0183(12) -0.0023(13) C11 0.0431(14) 0.0747(18) 0.0512(16) -0.0062(13) 0.0084(12) 0.0101(13) C12 0.0462(14) 0.0804(19) 0.0557(17) -0.0112(14) 0.0208(12) 0.0030(13) C13 0.0452(13) 0.0652(17) 0.0506(15) 0.0035(12) 0.0181(12) 0.0037(12) C14 0.0513(14) 0.0545(15) 0.0536(16) 0.0015(12) 0.0219(12) -0.0027(12) C15 0.0765(19) 0.093(2) 0.099(2) -0.0345(19) 0.0523(19) -0.0316(17) C16 0.106(3) 0.117(3) 0.119(3) -0.054(2) 0.078(2) -0.042(2) C17 0.097(2) 0.076(2) 0.084(2) -0.0254(17) 0.039(2) -0.0294(18) C18 0.0653(18) 0.0596(18) 0.081(2) -0.0020(15) 0.0186(16) -0.0127(14) C19 0.0528(15) 0.0587(16) 0.0666(18) 0.0049(14) 0.0242(13) 0.0021(13) C20 0.0474(14) 0.0537(16) 0.0607(18) 0.0022(13) 0.0194(13) 0.0003(12) C21 0.0549(15) 0.0560(16) 0.0660(19) -0.0009(14) 0.0208(14) -0.0003(12) C22 0.0616(16) 0.0546(16) 0.0638(19) -0.0004(13) 0.0271(14) -0.0047(13) C23 0.0471(14) 0.0707(19) 0.0588(18) 0.0086(14) 0.0203(13) -0.0041(13) C24 0.0649(18) 0.093(2) 0.067(2) 0.0129(17) 0.0222(16) -0.0125(16) C25 0.0609(19) 0.152(4) 0.064(2) 0.014(2) 0.0168(17) -0.005(2) C26 0.061(2) 0.171(4) 0.085(3) 0.046(3) 0.0200(19) 0.024(2) C27 0.0631(19) 0.107(3) 0.117(3) 0.030(2) 0.038(2) 0.0299(19) C28 0.0535(16) 0.091(2) 0.075(2) 0.0132(17) 0.0274(15) 0.0086(16) N1 0.0407(10) 0.0724(15) 0.0514(13) -0.0081(10) 0.0162(10) -0.0044(10) N2 0.0376(10) 0.0692(13) 0.0545(14) 0.0052(10) 0.0145(10) 0.0069(10) N3 0.0614(13) 0.0491(13) 0.0576(14) 0.0024(10) 0.0123(11) 0.0027(10) N4 0.0451(11) 0.0607(13) 0.0487(13) -0.0014(10) 0.0110(10) -0.0020(10) O1 0.0652(11) 0.0688(11) 0.0582(12) -0.0061(9) 0.0198(9) 0.0084(9) O2 0.0911(14) 0.0740(13) 0.0638(12) 0.0042(10) 0.0285(11) 0.0277(11) O3 0.0511(10) 0.1011(15) 0.0572(12) -0.0242(10) 0.0178(9) 0.0013(10) O4 0.0527(11) 0.0953(15) 0.0959(16) -0.0355(12) 0.0172(11) -0.0071(10) O5 0.0616(11) 0.0819(13) 0.0636(12) 0.0019(10) 0.0086(9) -0.0308(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O3 1.9307(17) . ? Zn1 O1 1.9546(18) . ? Zn1 N4 1.993(2) 3_656 ? Zn1 N1 2.0139(18) . ? C1 N1 1.307(3) . ? C1 N2 1.344(3) . ? C1 H1 0.9300 . ? C2 C3 1.344(3) . ? C2 N1 1.378(3) . ? C2 H2 0.9300 . ? C3 N2 1.362(3) . ? C3 H3 0.9300 . ? C4 N2 1.458(3) . ? C4 C5 1.486(4) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 O5 1.415(3) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 O5 1.404(3) . ? C6 C7 1.499(4) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 N3 1.460(3) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.339(3) . ? C8 N3 1.370(3) . ? C8 H8 0.9300 . ? C9 N4 1.373(3) . ? C9 H9 0.9300 . ? C10 N4 1.316(3) . ? C10 N3 1.338(3) . ? C10 H10 0.9300 . ? C11 O4 1.223(3) . ? C11 O3 1.280(3) . ? C11 C12 1.486(3) . ? C12 C13 1.309(3) . ? C12 H12 0.9300 . ? C13 C14 1.467(3) . ? C13 H13 0.9300 . ? C14 C15 1.381(3) . ? C14 C19 1.391(3) . ? C15 C16 1.382(4) . ? C15 H15 0.9300 . ? C16 C17 1.370(4) . ? C16 H16 0.9300 . ? C17 C18 1.351(4) . ? C17 H17 0.9300 . ? C18 C19 1.367(4) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C20 O2 1.232(3) . ? C20 O1 1.272(3) . ? C20 C21 1.492(3) . ? C21 C22 1.299(3) . ? C21 H21 0.9300 . ? C22 C23 1.473(4) . ? C22 H22 0.9300 . ? C23 C28 1.382(4) . ? C23 C24 1.384(4) . ? C24 C25 1.372(4) . ? C24 H24 0.9300 . ? C25 C26 1.348(5) . ? C25 H25 0.9300 . ? C26 C27 1.371(5) . ? C26 H26 0.9300 . ? C27 C28 1.401(4) . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? N4 Zn1 1.993(2) 3_656 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Zn1 O1 103.30(8) . . ? O3 Zn1 N4 118.83(8) . 3_656 ? O1 Zn1 N4 112.09(7) . 3_656 ? O3 Zn1 N1 101.06(7) . . ? O1 Zn1 N1 114.21(8) . . ? N4 Zn1 N1 107.14(8) 3_656 . ? N1 C1 N2 111.4(2) . . ? N1 C1 H1 124.3 . . ? N2 C1 H1 124.3 . . ? C3 C2 N1 109.6(2) . . ? C3 C2 H2 125.2 . . ? N1 C2 H2 125.2 . . ? C2 C3 N2 106.4(2) . . ? C2 C3 H3 126.8 . . ? N2 C3 H3 126.8 . . ? N2 C4 C5 112.5(2) . . ? N2 C4 H4A 109.1 . . ? C5 C4 H4A 109.1 . . ? N2 C4 H4B 109.1 . . ? C5 C4 H4B 109.1 . . ? H4A C4 H4B 107.8 . . ? O5 C5 C4 107.5(2) . . ? O5 C5 H5A 110.2 . . ? C4 C5 H5A 110.2 . . ? O5 C5 H5B 110.2 . . ? C4 C5 H5B 110.2 . . ? H5A C5 H5B 108.5 . . ? O5 C6 C7 107.3(2) . . ? O5 C6 H6A 110.3 . . ? C7 C6 H6A 110.3 . . ? O5 C6 H6B 110.3 . . ? C7 C6 H6B 110.3 . . ? H6A C6 H6B 108.5 . . ? N3 C7 C6 111.1(2) . . ? N3 C7 H7A 109.4 . . ? C6 C7 H7A 109.4 . . ? N3 C7 H7B 109.4 . . ? C6 C7 H7B 109.4 . . ? H7A C7 H7B 108.0 . . ? C9 C8 N3 106.9(2) . . ? C9 C8 H8 126.6 . . ? N3 C8 H8 126.6 . . ? C8 C9 N4 109.5(2) . . ? C8 C9 H9 125.3 . . ? N4 C9 H9 125.3 . . ? N4 C10 N3 111.6(2) . . ? N4 C10 H10 124.2 . . ? N3 C10 H10 124.2 . . ? O4 C11 O3 124.6(2) . . ? O4 C11 C12 120.0(2) . . ? O3 C11 C12 115.3(2) . . ? C13 C12 C11 124.0(2) . . ? C13 C12 H12 118.0 . . ? C11 C12 H12 118.0 . . ? C12 C13 C14 128.6(2) . . ? C12 C13 H13 115.7 . . ? C14 C13 H13 115.7 . . ? C15 C14 C19 116.9(2) . . ? C15 C14 C13 123.7(2) . . ? C19 C14 C13 119.4(2) . . ? C14 C15 C16 120.7(3) . . ? C14 C15 H15 119.7 . . ? C16 C15 H15 119.7 . . ? C17 C16 C15 120.4(3) . . ? C17 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? C18 C17 C16 119.9(3) . . ? C18 C17 H17 120.1 . . ? C16 C17 H17 120.1 . . ? C17 C18 C19 120.0(3) . . ? C17 C18 H18 120.0 . . ? C19 C18 H18 120.0 . . ? C18 C19 C14 122.1(2) . . ? C18 C19 H19 119.0 . . ? C14 C19 H19 119.0 . . ? O2 C20 O1 124.5(2) . . ? O2 C20 C21 120.8(2) . . ? O1 C20 C21 114.7(2) . . ? C22 C21 C20 123.6(2) . . ? C22 C21 H21 118.2 . . ? C20 C21 H21 118.2 . . ? C21 C22 C23 128.2(3) . . ? C21 C22 H22 115.9 . . ? C23 C22 H22 115.9 . . ? C28 C23 C24 118.5(3) . . ? C28 C23 C22 122.9(3) . . ? C24 C23 C22 118.6(3) . . ? C25 C24 C23 121.1(3) . . ? C25 C24 H24 119.4 . . ? C23 C24 H24 119.4 . . ? C26 C25 C24 120.1(4) . . ? C26 C25 H25 120.0 . . ? C24 C25 H25 120.0 . . ? C25 C26 C27 121.0(4) . . ? C25 C26 H26 119.5 . . ? C27 C26 H26 119.5 . . ? C26 C27 C28 119.3(3) . . ? C26 C27 H27 120.3 . . ? C28 C27 H27 120.3 . . ? C23 C28 C27 120.0(3) . . ? C23 C28 H28 120.0 . . ? C27 C28 H28 120.0 . . ? C1 N1 C2 105.5(2) . . ? C1 N1 Zn1 127.61(17) . . ? C2 N1 Zn1 126.92(17) . . ? C1 N2 C3 107.1(2) . . ? C1 N2 C4 126.1(2) . . ? C3 N2 C4 126.7(2) . . ? C10 N3 C8 106.6(2) . . ? C10 N3 C7 125.6(2) . . ? C8 N3 C7 127.3(2) . . ? C10 N4 C9 105.5(2) . . ? C10 N4 Zn1 125.39(17) . 3_656 ? C9 N4 Zn1 129.02(18) . 3_656 ? C20 O1 Zn1 116.02(16) . . ? C11 O3 Zn1 119.74(16) . . ? C6 O5 C5 114.8(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C2 C3 N2 0.1(3) . . . . ? N2 C4 C5 O5 -63.8(3) . . . . ? O5 C6 C7 N3 -61.6(3) . . . . ? N3 C8 C9 N4 -0.8(3) . . . . ? O4 C11 C12 C13 -170.7(3) . . . . ? O3 C11 C12 C13 8.1(4) . . . . ? C11 C12 C13 C14 -178.8(2) . . . . ? C12 C13 C14 C15 -9.6(4) . . . . ? C12 C13 C14 C19 170.5(3) . . . . ? C19 C14 C15 C16 -1.3(5) . . . . ? C13 C14 C15 C16 178.7(3) . . . . ? C14 C15 C16 C17 -0.1(6) . . . . ? C15 C16 C17 C18 1.5(6) . . . . ? C16 C17 C18 C19 -1.4(5) . . . . ? C17 C18 C19 C14 0.0(4) . . . . ? C15 C14 C19 C18 1.4(4) . . . . ? C13 C14 C19 C18 -178.7(2) . . . . ? O2 C20 C21 C22 8.5(4) . . . . ? O1 C20 C21 C22 -170.8(2) . . . . ? C20 C21 C22 C23 178.2(2) . . . . ? C21 C22 C23 C28 13.8(4) . . . . ? C21 C22 C23 C24 -168.2(3) . . . . ? C28 C23 C24 C25 1.9(4) . . . . ? C22 C23 C24 C25 -176.2(2) . . . . ? C23 C24 C25 C26 0.6(4) . . . . ? C24 C25 C26 C27 -2.1(5) . . . . ? C25 C26 C27 C28 1.1(5) . . . . ? C24 C23 C28 C27 -2.8(4) . . . . ? C22 C23 C28 C27 175.2(2) . . . . ? C26 C27 C28 C23 1.4(4) . . . . ? N2 C1 N1 C2 0.6(3) . . . . ? N2 C1 N1 Zn1 -178.29(16) . . . . ? C3 C2 N1 C1 -0.4(3) . . . . ? C3 C2 N1 Zn1 178.47(18) . . . . ? O3 Zn1 N1 C1 -166.0(2) . . . . ? O1 Zn1 N1 C1 -55.8(2) . . . . ? N4 Zn1 N1 C1 68.9(2) 3_656 . . . ? O3 Zn1 N1 C2 15.4(2) . . . . ? O1 Zn1 N1 C2 125.6(2) . . . . ? N4 Zn1 N1 C2 -109.7(2) 3_656 . . . ? N1 C1 N2 C3 -0.5(3) . . . . ? N1 C1 N2 C4 -177.7(2) . . . . ? C2 C3 N2 C1 0.2(3) . . . . ? C2 C3 N2 C4 177.4(2) . . . . ? C5 C4 N2 C1 78.0(3) . . . . ? C5 C4 N2 C3 -98.6(3) . . . . ? N4 C10 N3 C8 -0.5(3) . . . . ? N4 C10 N3 C7 -172.5(2) . . . . ? C9 C8 N3 C10 0.8(3) . . . . ? C9 C8 N3 C7 172.6(2) . . . . ? C6 C7 N3 C10 94.8(3) . . . . ? C6 C7 N3 C8 -75.5(3) . . . . ? N3 C10 N4 C9 0.0(3) . . . . ? N3 C10 N4 Zn1 176.96(15) . . . 3_656 ? C8 C9 N4 C10 0.5(3) . . . . ? C8 C9 N4 Zn1 -176.29(16) . . . 3_656 ? O2 C20 O1 Zn1 -8.5(3) . . . . ? C21 C20 O1 Zn1 170.70(15) . . . . ? O3 Zn1 O1 C20 172.93(16) . . . . ? N4 Zn1 O1 C20 -57.97(18) 3_656 . . . ? N1 Zn1 O1 C20 64.12(18) . . . . ? O4 C11 O3 Zn1 14.9(4) . . . . ? C12 C11 O3 Zn1 -163.78(17) . . . . ? O1 Zn1 O3 C11 74.8(2) . . . . ? N4 Zn1 O3 C11 -50.0(2) 3_656 . . . ? N1 Zn1 O3 C11 -166.78(19) . . . . ? C7 C6 O5 C5 -174.2(2) . . . . ? C4 C5 O5 C6 164.8(2) . . . . ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.261 _refine_diff_density_min -0.252 _refine_diff_density_rms 0.053 #===END data_compound2 _database_code_depnum_ccdc_archive 'CCDC 665625' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H16 N4 O6 Zn' _chemical_formula_sum 'C12 H16 N4 O6 Zn' _chemical_formula_weight 377.66 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 2/n' _symmetry_space_group_name_Hall '-P 2yac' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z-1/2' _cell_length_a 11.876(4) _cell_length_b 10.864(5) _cell_length_c 11.960(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.869(13) _cell_angle_gamma 90.00 _cell_volume 1542.9(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2093 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.626 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 776 _exptl_absorpt_coefficient_mu 1.628 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.830 _exptl_absorpt_correction_T_max 0.850 _exptl_absorpt_process_details ; Higashi,T (1995) Program for absorption correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14593 _diffrn_reflns_av_R_equivalents 0.0672 _diffrn_reflns_av_sigmaI/netI 0.0592 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 27.46 _reflns_number_total 3508 _reflns_number_gt 2093 _reflns_threshold_expression >2sigma(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction PROCESS-AUTO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0692P)^2^+1.9599P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0088(16) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3508 _refine_ls_number_parameters 210 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1063 _refine_ls_R_factor_gt 0.0553 _refine_ls_wR_factor_ref 0.1618 _refine_ls_wR_factor_gt 0.1325 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn -0.02567(5) 0.35614(5) 0.68879(4) 0.0446(2) Uani 1 1 d . . . C1 C 0.0951(5) 0.1652(5) 0.5403(5) 0.0621(15) Uani 1 1 d . . . H1 H 0.0841 0.2120 0.4759 0.075 Uiso 1 1 calc R . . C2 C 0.1426(6) 0.0142(6) 0.6481(5) 0.085(2) Uani 1 1 d . . . H2 H 0.1694 -0.0608 0.6749 0.102 Uiso 1 1 calc R . . C3 C 0.0994(6) 0.1074(6) 0.7086(5) 0.0766(18) Uani 1 1 d . . . H3 H 0.0914 0.1065 0.7859 0.092 Uiso 1 1 calc R . . C4 C 0.1779(5) -0.0179(7) 0.4429(6) 0.084(2) Uani 1 1 d . . . H4A H 0.1367 0.0100 0.3769 0.100 Uiso 1 1 calc R . . H4B H 0.1606 -0.1043 0.4537 0.100 Uiso 1 1 calc R . . C5 C 0.3004(6) -0.0047(6) 0.4233(6) 0.0818(19) Uani 1 1 d . . . H5A H 0.3429 -0.0275 0.4900 0.098 Uiso 1 1 calc R . . H5B H 0.3231 -0.0578 0.3625 0.098 Uiso 1 1 calc R . . C6 C 0.4159(9) 0.1532(8) 0.3583(7) 0.119(3) Uani 1 1 d . . . H6A H 0.4194 0.1258 0.2813 0.143 Uiso 1 1 calc R . . H6B H 0.4737 0.1086 0.3997 0.143 Uiso 1 1 calc R . . C7 C 0.4466(5) 0.2819(6) 0.3603(4) 0.0682(16) Uani 1 1 d D . . H7A H 0.4017 0.3260 0.3050 0.082 Uiso 1 1 calc R . . H7B H 0.5252 0.2903 0.3407 0.082 Uiso 1 1 calc R . . C8 C 0.3371(5) 0.3936(6) 0.5086(5) 0.0743(18) Uani 1 1 d . . . H8 H 0.2734 0.4151 0.4667 0.089 Uiso 1 1 calc R . . C9 C 0.3543(5) 0.4140(6) 0.6188(5) 0.0728(17) Uani 1 1 d . . . H9 H 0.3038 0.4528 0.6660 0.087 Uiso 1 1 calc R . . C10 C 0.4996(4) 0.3234(5) 0.5591(4) 0.0520(12) Uani 1 1 d . . . H10 H 0.5701 0.2864 0.5557 0.062 Uiso 1 1 calc R . . C11 C -0.2500 0.4332(6) 0.7500 0.0414(14) Uani 1 2 d S . . C12 C -0.2500 0.2902(6) 0.7500 0.0386(14) Uani 1 2 d S . . C13 C -0.0454(4) 0.4625(4) 0.4673(4) 0.0443(11) Uani 1 1 d . . . N1 N 0.0693(3) 0.2026(4) 0.6409(3) 0.0513(10) Uani 1 1 d . . . N2 N 0.1390(4) 0.0524(4) 0.5410(4) 0.0656(13) Uani 1 1 d . . . N3 N 0.4290(4) 0.3364(4) 0.4709(3) 0.0503(10) Uani 1 1 d . . . N4 N 0.4569(4) 0.3692(4) 0.6502(3) 0.0484(10) Uani 1 1 d . . . O1 O -0.0845(3) 0.3691(3) 0.5147(3) 0.0547(9) Uani 1 1 d . . . O2 O -0.0720(3) 0.4993(3) 0.3713(3) 0.0513(8) Uani 1 1 d . . . O3 O -0.1602(3) 0.4846(3) 0.7224(3) 0.0535(9) Uani 1 1 d . . . O4 O -0.1587(3) 0.2380(3) 0.7309(3) 0.0453(8) Uani 1 1 d . . . O5 O 0.3210(6) 0.1194(5) 0.3960(5) 0.121(2) Uani 1 1 d . . . O1W O 0.7389(5) 0.2738(7) 0.3760(7) 0.178(3) Uani 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0467(4) 0.0432(4) 0.0439(4) 0.0056(2) 0.0039(2) -0.0033(3) C1 0.070(4) 0.058(4) 0.059(3) -0.009(3) 0.006(3) 0.009(3) C2 0.109(6) 0.066(4) 0.079(5) -0.004(3) -0.007(4) 0.032(4) C3 0.090(5) 0.075(4) 0.065(4) -0.004(3) 0.000(3) 0.029(4) C4 0.069(4) 0.087(5) 0.094(5) -0.046(4) -0.003(3) 0.003(4) C5 0.089(5) 0.065(4) 0.092(5) -0.033(4) 0.008(4) 0.002(4) C6 0.152(9) 0.120(7) 0.086(6) -0.051(5) 0.031(5) -0.046(6) C7 0.085(4) 0.076(4) 0.044(3) -0.009(3) 0.005(3) 0.008(3) C8 0.070(4) 0.096(5) 0.056(4) -0.004(3) -0.011(3) 0.035(4) C9 0.064(4) 0.098(5) 0.057(3) -0.003(3) 0.006(3) 0.031(4) C10 0.046(3) 0.057(3) 0.053(3) -0.008(2) 0.002(2) 0.004(2) C11 0.046(4) 0.033(3) 0.045(3) 0.000 -0.005(3) 0.000 C12 0.043(4) 0.037(4) 0.035(3) 0.000 0.002(2) 0.000 C13 0.040(3) 0.049(3) 0.045(3) 0.002(2) 0.0062(19) 0.002(2) N1 0.050(3) 0.049(3) 0.055(3) -0.0020(19) 0.0021(18) 0.004(2) N2 0.055(3) 0.063(3) 0.079(3) -0.026(2) -0.008(2) 0.008(2) N3 0.060(3) 0.050(3) 0.040(2) -0.0017(17) 0.0011(18) 0.001(2) N4 0.053(3) 0.051(3) 0.041(2) -0.0009(17) 0.0043(17) 0.0031(19) O1 0.058(2) 0.053(2) 0.053(2) 0.0134(16) -0.0028(15) -0.0143(17) O2 0.049(2) 0.056(2) 0.0493(19) 0.0124(15) -0.0003(14) -0.0080(16) O3 0.049(2) 0.0347(18) 0.077(2) 0.0033(16) 0.0086(17) -0.0033(15) O4 0.0446(19) 0.0316(17) 0.060(2) 0.0010(14) 0.0095(14) 0.0023(14) O5 0.140(5) 0.080(4) 0.146(5) -0.045(3) 0.069(4) -0.020(3) O1W 0.105(5) 0.138(6) 0.287(10) -0.034(6) -0.060(6) 0.003(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N4 2.085(4) 2_556 ? Zn1 O2 2.086(3) 3_566 ? Zn1 N1 2.098(4) . ? Zn1 O4 2.102(3) . ? Zn1 O3 2.164(3) . ? Zn1 O1 2.191(3) . ? C1 N1 1.311(6) . ? C1 N2 1.332(7) . ? C1 H1 0.9300 . ? C2 N2 1.347(8) . ? C2 C3 1.350(8) . ? C2 H2 0.9300 . ? C3 N1 1.359(7) . ? C3 H3 0.9300 . ? C4 N2 1.479(7) . ? C4 C5 1.484(9) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 O5 1.410(8) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 O5 1.275(10) . ? C6 C7 1.444(9) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 N3 1.467(6) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 N3 1.340(7) . ? C8 C9 1.349(8) . ? C8 H8 0.9300 . ? C9 N4 1.360(7) . ? C9 H9 0.9300 . ? C10 N4 1.308(6) . ? C10 N3 1.345(6) . ? C10 H10 0.9300 . ? C11 O3 1.252(4) . ? C11 O3 1.252(4) 2_456 ? C11 C12 1.553(9) . ? C12 O4 1.248(4) 2_456 ? C12 O4 1.248(4) . ? C13 O2 1.253(5) . ? C13 O1 1.255(5) . ? C13 C13 1.553(9) 3_566 ? N4 Zn1 2.085(4) 2_556 ? O2 Zn1 2.086(3) 3_566 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Zn1 O2 93.13(14) 2_556 3_566 ? N4 Zn1 N1 95.83(16) 2_556 . ? O2 Zn1 N1 101.57(16) 3_566 . ? N4 Zn1 O4 96.07(14) 2_556 . ? O2 Zn1 O4 164.94(13) 3_566 . ? N1 Zn1 O4 89.35(14) . . ? N4 Zn1 O3 93.69(15) 2_556 . ? O2 Zn1 O3 89.71(13) 3_566 . ? N1 Zn1 O3 164.78(15) . . ? O4 Zn1 O3 77.84(12) . . ? N4 Zn1 O1 171.20(14) 2_556 . ? O2 Zn1 O1 78.20(12) 3_566 . ? N1 Zn1 O1 87.50(15) . . ? O4 Zn1 O1 92.10(12) . . ? O3 Zn1 O1 84.82(14) . . ? N1 C1 N2 112.1(5) . . ? N1 C1 H1 124.0 . . ? N2 C1 H1 124.0 . . ? N2 C2 C3 105.8(6) . . ? N2 C2 H2 127.1 . . ? C3 C2 H2 127.1 . . ? C2 C3 N1 110.5(6) . . ? C2 C3 H3 124.8 . . ? N1 C3 H3 124.8 . . ? N2 C4 C5 113.2(5) . . ? N2 C4 H4A 108.9 . . ? C5 C4 H4A 108.9 . . ? N2 C4 H4B 108.9 . . ? C5 C4 H4B 108.9 . . ? H4A C4 H4B 107.8 . . ? O5 C5 C4 107.6(6) . . ? O5 C5 H5A 110.2 . . ? C4 C5 H5A 110.2 . . ? O5 C5 H5B 110.2 . . ? C4 C5 H5B 110.2 . . ? H5A C5 H5B 108.5 . . ? O5 C6 C7 119.8(8) . . ? O5 C6 H6A 107.4 . . ? C7 C6 H6A 107.4 . . ? O5 C6 H6B 107.4 . . ? C7 C6 H6B 107.4 . . ? H6A C6 H6B 106.9 . . ? C6 C7 N3 111.5(5) . . ? C6 C7 H7A 109.3 . . ? N3 C7 H7A 109.3 . . ? C6 C7 H7B 109.3 . . ? N3 C7 H7B 109.3 . . ? H7A C7 H7B 108.0 . . ? N3 C8 C9 107.0(5) . . ? N3 C8 H8 126.5 . . ? C9 C8 H8 126.5 . . ? C8 C9 N4 109.5(5) . . ? C8 C9 H9 125.3 . . ? N4 C9 H9 125.3 . . ? N4 C10 N3 111.6(5) . . ? N4 C10 H10 124.2 . . ? N3 C10 H10 124.2 . . ? O3 C11 O3 127.0(6) . 2_456 ? O3 C11 C12 116.5(3) . . ? O3 C11 C12 116.5(3) 2_456 . ? O4 C12 O4 125.9(6) 2_456 . ? O4 C12 C11 117.0(3) 2_456 . ? O4 C12 C11 117.0(3) . . ? O2 C13 O1 125.6(4) . . ? O2 C13 C13 117.2(5) . 3_566 ? O1 C13 C13 117.1(5) . 3_566 ? C1 N1 C3 104.4(5) . . ? C1 N1 Zn1 129.1(4) . . ? C3 N1 Zn1 125.5(4) . . ? C1 N2 C2 107.2(5) . . ? C1 N2 C4 126.6(6) . . ? C2 N2 C4 126.2(6) . . ? C8 N3 C10 106.7(4) . . ? C8 N3 C7 128.2(5) . . ? C10 N3 C7 124.7(5) . . ? C10 N4 C9 105.3(4) . . ? C10 N4 Zn1 126.3(4) . 2_556 ? C9 N4 Zn1 128.0(3) . 2_556 ? C13 O1 Zn1 111.5(3) . . ? C13 O2 Zn1 115.0(3) . 3_566 ? C11 O3 Zn1 113.3(3) . . ? C12 O4 Zn1 115.1(3) . . ? C6 O5 C5 121.0(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 C2 C3 N1 -0.1(8) . . . . ? N2 C4 C5 O5 -64.9(8) . . . . ? O5 C6 C7 N3 49.5(11) . . . . ? N3 C8 C9 N4 -0.2(8) . . . . ? O3 C11 C12 O4 -174.8(2) . . . 2_456 ? O3 C11 C12 O4 5.2(2) 2_456 . . 2_456 ? O3 C11 C12 O4 5.2(2) . . . . ? O3 C11 C12 O4 -174.8(2) 2_456 . . . ? N2 C1 N1 C3 0.3(7) . . . . ? N2 C1 N1 Zn1 -168.6(4) . . . . ? C2 C3 N1 C1 -0.1(8) . . . . ? C2 C3 N1 Zn1 169.3(5) . . . . ? N4 Zn1 N1 C1 -157.1(5) 2_556 . . . ? O2 Zn1 N1 C1 -62.7(5) 3_566 . . . ? O4 Zn1 N1 C1 106.9(5) . . . . ? O3 Zn1 N1 C1 74.5(8) . . . . ? O1 Zn1 N1 C1 14.7(5) . . . . ? N4 Zn1 N1 C3 36.2(5) 2_556 . . . ? O2 Zn1 N1 C3 130.6(5) 3_566 . . . ? O4 Zn1 N1 C3 -59.9(5) . . . . ? O3 Zn1 N1 C3 -92.3(7) . . . . ? O1 Zn1 N1 C3 -152.0(5) . . . . ? N1 C1 N2 C2 -0.4(7) . . . . ? N1 C1 N2 C4 -179.8(5) . . . . ? C3 C2 N2 C1 0.2(8) . . . . ? C3 C2 N2 C4 179.7(6) . . . . ? C5 C4 N2 C1 94.7(8) . . . . ? C5 C4 N2 C2 -84.7(9) . . . . ? C9 C8 N3 C10 0.0(7) . . . . ? C9 C8 N3 C7 172.3(6) . . . . ? N4 C10 N3 C8 0.1(6) . . . . ? N4 C10 N3 C7 -172.5(5) . . . . ? C6 C7 N3 C8 -91.7(8) . . . . ? C6 C7 N3 C10 79.3(8) . . . . ? N3 C10 N4 C9 -0.2(6) . . . . ? N3 C10 N4 Zn1 173.4(3) . . . 2_556 ? C8 C9 N4 C10 0.3(7) . . . . ? C8 C9 N4 Zn1 -173.2(4) . . . 2_556 ? O2 C13 O1 Zn1 -173.4(4) . . . . ? C13 C13 O1 Zn1 7.7(6) 3_566 . . . ? O2 Zn1 O1 C13 -8.5(3) 3_566 . . . ? N1 Zn1 O1 C13 -110.9(3) . . . . ? O4 Zn1 O1 C13 159.9(3) . . . . ? O3 Zn1 O1 C13 82.3(3) . . . . ? O1 C13 O2 Zn1 -172.1(4) . . . 3_566 ? C13 C13 O2 Zn1 6.9(6) 3_566 . . 3_566 ? O3 C11 O3 Zn1 177.5(3) 2_456 . . . ? C12 C11 O3 Zn1 -2.5(3) . . . . ? N4 Zn1 O3 C11 -95.3(2) 2_556 . . . ? O2 Zn1 O3 C11 171.6(2) 3_566 . . . ? N1 Zn1 O3 C11 33.4(7) . . . . ? O4 Zn1 O3 C11 0.1(2) . . . . ? O1 Zn1 O3 C11 93.4(2) . . . . ? O4 C12 O4 Zn1 175.0(2) 2_456 . . . ? C11 C12 O4 Zn1 -5.0(2) . . . . ? N4 Zn1 O4 C12 95.4(2) 2_556 . . . ? O2 Zn1 O4 C12 -32.0(6) 3_566 . . . ? N1 Zn1 O4 C12 -168.9(2) . . . . ? O3 Zn1 O4 C12 2.9(2) . . . . ? O1 Zn1 O4 C12 -81.4(2) . . . . ? C7 C6 O5 C5 -162.8(7) . . . . ? C4 C5 O5 C6 -169.1(7) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.859 _refine_diff_density_min -0.751 _refine_diff_density_rms 0.091 #===END data_compound3 _database_code_depnum_ccdc_archive 'CCDC 665626' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H36 N8 O10 Zn2' _chemical_formula_sum 'C36 H36 N8 O10 Zn2' _chemical_formula_weight 871.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C c' _symmetry_space_group_name_Hall 'C -2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 14.675(8) _cell_length_b 9.636(4) _cell_length_c 13.262(6) _cell_angle_alpha 90.00 _cell_angle_beta 97.17(2) _cell_angle_gamma 90.00 _cell_volume 1860.7(15) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.490 _exptl_crystal_size_mid 0.477 _exptl_crystal_size_min 0.055 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.555 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 896 _exptl_absorpt_coefficient_mu 1.358 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8977 _exptl_absorpt_correction_T_max 1.1170 _exptl_absorpt_process_details ; Higashi,T (1995) Program for absorption correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8934 _diffrn_reflns_av_R_equivalents 0.0256 _diffrn_reflns_av_sigmaI/netI 0.0448 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 27.47 _reflns_number_total 3784 _reflns_number_gt 3479 _reflns_threshold_expression >2sigma(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction PROCESS-AUTO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0324P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.012(9) _refine_ls_number_reflns 3784 _refine_ls_number_parameters 253 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0305 _refine_ls_R_factor_gt 0.0267 _refine_ls_wR_factor_ref 0.0617 _refine_ls_wR_factor_gt 0.0600 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.044969(18) 0.43983(2) 0.302067(19) 0.03434(8) Uani 1 1 d . . . C1 C -0.09961(18) 0.4928(3) 0.4382(2) 0.0456(6) Uani 1 1 d . . . H1 H -0.0642 0.5600 0.4750 0.055 Uiso 1 1 calc R . . C2 C -0.1465(2) 0.3388(3) 0.3275(2) 0.0588(8) Uani 1 1 d . . . H2 H -0.1490 0.2796 0.2719 0.071 Uiso 1 1 calc R . . C3 C -0.2113(2) 0.3504(4) 0.3893(3) 0.0656(9) Uani 1 1 d . . . H3 H -0.2659 0.3004 0.3854 0.079 Uiso 1 1 calc R . . C4 C -0.2250(3) 0.4902(3) 0.5489(3) 0.0739(11) Uani 1 1 d . . . H4A H -0.2912 0.4897 0.5316 0.089 Uiso 1 1 calc R . . H4B H -0.2065 0.5841 0.5682 0.089 Uiso 1 1 calc R . . C5 C -0.2001(3) 0.3973(4) 0.6363(3) 0.0727(11) Uani 1 1 d . . . H5A H -0.1338 0.3910 0.6508 0.087 Uiso 1 1 calc R . . H5B H -0.2237 0.4346 0.6959 0.087 Uiso 1 1 calc R . . C6 C -0.1823(2) 0.1575(4) 0.6633(3) 0.0660(9) Uani 1 1 d . . . H6A H -0.1610 0.1843 0.7327 0.079 Uiso 1 1 calc R . . H6B H -0.1291 0.1418 0.6281 0.079 Uiso 1 1 calc R . . C7 C -0.2368(3) 0.0322(5) 0.6623(4) 0.0755(13) Uani 1 1 d . . . H7A H -0.2913 0.0517 0.6944 0.091 Uiso 1 1 calc R . . H7B H -0.2017 -0.0378 0.7028 0.091 Uiso 1 1 calc R . . C8 C -0.2247(2) -0.1296(3) 0.5123(3) 0.0604(8) Uani 1 1 d . . . H8 H -0.1708 -0.1761 0.5362 0.072 Uiso 1 1 calc R . . C9 C -0.2776(2) -0.1520(3) 0.4245(2) 0.0533(7) Uani 1 1 d . . . H9 H -0.2671 -0.2191 0.3768 0.064 Uiso 1 1 calc R . . C10 C -0.33961(19) 0.0140(3) 0.4990(2) 0.0446(6) Uani 1 1 d . . . H10 H -0.3791 0.0848 0.5132 0.054 Uiso 1 1 calc R . . C11 C 0.05823(17) 0.7097(2) 0.2445(2) 0.0320(5) Uani 1 1 d . . . C12 C 0.05316(15) 0.8269(2) 0.16848(17) 0.0288(4) Uani 1 1 d . . . C13 C 0.04245(17) 0.7992(2) 0.0652(2) 0.0357(5) Uani 1 1 d . . . H13 H 0.0452 0.7081 0.0426 0.043 Uiso 1 1 calc R . . C14 C 0.0276(2) 0.9066(3) -0.0047(2) 0.0415(7) Uani 1 1 d . . . H14 H 0.0220 0.8873 -0.0739 0.050 Uiso 1 1 calc R . . C15 C 0.02124(19) 1.0420(2) 0.02811(19) 0.0384(5) Uani 1 1 d . . . H15 H 0.0084 1.1133 -0.0188 0.046 Uiso 1 1 calc R . . C16 C 0.03402(18) 1.0712(2) 0.1316(2) 0.0308(6) Uani 1 1 d . . . C17 C 0.05194(16) 0.9642(2) 0.20176(18) 0.0293(4) Uani 1 1 d . . . H17 H 0.0631 0.9842 0.2708 0.035 Uiso 1 1 calc R . . C18 C 0.02328(17) 1.2183(2) 0.16686(18) 0.0354(5) Uani 1 1 d . . . N1 N -0.07536(16) 0.42783(19) 0.35863(18) 0.0425(5) Uani 1 1 d . . . N2 N -0.1819(2) 0.4498(3) 0.4594(3) 0.0552(9) Uani 1 1 d . . . N3 N -0.26530(18) -0.0247(2) 0.56050(19) 0.0542(6) Uani 1 1 d . . . N4 N -0.34985(16) -0.06102(18) 0.41538(17) 0.0392(5) Uani 1 1 d . . . O1 O 0.05665(15) 0.58816(15) 0.20559(14) 0.0450(4) Uani 1 1 d . . . O2 O 0.05973(16) 0.73318(19) 0.33525(15) 0.0531(6) Uani 1 1 d . . . O3 O -0.02729(16) 1.29822(18) 0.11366(16) 0.0600(6) Uani 1 1 d . . . O4 O 0.06638(14) 1.25002(15) 0.25359(14) 0.0440(4) Uani 1 1 d . . . O5 O -0.23748(16) 0.2637(2) 0.61433(19) 0.0634(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.04779(15) 0.01921(10) 0.03462(13) 0.00113(15) -0.00039(9) -0.00293(14) C1 0.0413(15) 0.0326(12) 0.0621(17) -0.0072(13) 0.0036(13) -0.0049(10) C2 0.067(2) 0.0577(17) 0.0485(16) -0.0037(14) -0.0058(15) -0.0273(14) C3 0.054(2) 0.073(2) 0.069(2) 0.0034(19) 0.0005(17) -0.0269(16) C4 0.068(2) 0.0429(16) 0.119(3) -0.004(2) 0.045(2) 0.0074(15) C5 0.084(3) 0.062(2) 0.077(2) -0.0315(19) 0.027(2) -0.0223(17) C6 0.059(2) 0.072(2) 0.062(2) -0.0120(18) -0.0102(17) -0.0064(16) C7 0.091(3) 0.075(2) 0.052(2) 0.008(2) -0.025(2) -0.019(2) C8 0.0471(17) 0.0494(16) 0.079(2) 0.0163(16) -0.0124(16) 0.0046(13) C9 0.0594(18) 0.0405(14) 0.0591(18) 0.0030(13) 0.0043(14) 0.0077(12) C10 0.0482(16) 0.0345(11) 0.0479(15) 0.0002(12) -0.0072(12) -0.0018(11) C11 0.0389(13) 0.0217(10) 0.0356(14) -0.0003(10) 0.0057(11) 0.0012(9) C12 0.0305(11) 0.0215(9) 0.0345(12) -0.0019(9) 0.0048(9) 0.0000(8) C13 0.0462(14) 0.0243(10) 0.0375(13) -0.0050(10) 0.0092(10) 0.0003(9) C14 0.064(2) 0.0309(13) 0.0311(14) -0.0011(11) 0.0102(13) -0.0011(12) C15 0.0511(15) 0.0286(11) 0.0353(13) 0.0043(10) 0.0041(11) -0.0004(9) C16 0.0359(14) 0.0209(11) 0.0351(15) 0.0025(9) 0.0028(10) -0.0024(8) C17 0.0351(12) 0.0210(9) 0.0311(11) -0.0006(9) 0.0016(9) -0.0008(8) C18 0.0510(15) 0.0185(9) 0.0367(13) 0.0008(9) 0.0050(11) -0.0042(9) N1 0.0439(12) 0.0334(10) 0.0485(13) 0.0014(9) -0.0014(10) -0.0066(8) N2 0.0451(16) 0.0437(15) 0.077(2) 0.0027(13) 0.0074(15) -0.0009(10) N3 0.0639(16) 0.0397(11) 0.0524(14) 0.0077(11) -0.0186(12) -0.0077(11) N4 0.0458(12) 0.0281(9) 0.0422(12) 0.0040(8) 0.0001(9) -0.0020(8) O1 0.0758(14) 0.0174(7) 0.0418(10) 0.0022(7) 0.0074(9) -0.0008(7) O2 0.0946(18) 0.0283(9) 0.0366(11) 0.0038(8) 0.0091(11) 0.0045(10) O3 0.0926(16) 0.0261(8) 0.0550(12) 0.0003(8) -0.0158(11) 0.0135(9) O4 0.0665(12) 0.0236(8) 0.0397(9) -0.0045(7) -0.0013(8) 0.0002(7) O5 0.0653(14) 0.0513(11) 0.0708(15) -0.0063(11) -0.0023(11) -0.0149(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O1 1.9401(18) . ? Zn1 O4 1.9768(17) 1_545 ? Zn1 N1 2.006(3) . ? Zn1 N4 2.015(2) 3 ? C1 N1 1.313(4) . ? C1 N2 1.340(4) . ? C1 H1 0.9300 . ? C2 C3 1.336(5) . ? C2 N1 1.374(3) . ? C2 H2 0.9300 . ? C3 N2 1.367(5) . ? C3 H3 0.9300 . ? C4 N2 1.465(5) . ? C4 C5 1.474(6) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 O5 1.415(4) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 O5 1.412(4) . ? C6 C7 1.448(5) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 N3 1.469(5) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.335(5) . ? C8 N3 1.371(4) . ? C8 H8 0.9300 . ? C9 N4 1.369(3) . ? C9 H9 0.9300 . ? C10 N4 1.316(4) . ? C10 N3 1.331(4) . ? C10 H10 0.9300 . ? C11 O2 1.221(3) . ? C11 O1 1.279(3) . ? C11 C12 1.510(3) . ? C12 C13 1.385(3) . ? C12 C17 1.395(3) . ? C13 C14 1.388(4) . ? C13 H13 0.9300 . ? C14 C15 1.383(4) . ? C14 H14 0.9300 . ? C15 C16 1.391(4) . ? C15 H15 0.9300 . ? C16 C17 1.392(3) . ? C16 C18 1.507(3) . ? C17 H17 0.9300 . ? C18 O3 1.229(3) . ? C18 O4 1.279(3) . ? N4 Zn1 2.015(2) 3_445 ? O4 Zn1 1.9768(17) 1_565 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zn1 O4 115.88(8) . 1_545 ? O1 Zn1 N1 116.32(9) . . ? O4 Zn1 N1 104.55(8) 1_545 . ? O1 Zn1 N4 111.86(9) . 3 ? O4 Zn1 N4 95.78(8) 1_545 3 ? N1 Zn1 N4 110.42(10) . 3 ? N1 C1 N2 111.3(3) . . ? N1 C1 H1 124.3 . . ? N2 C1 H1 124.3 . . ? C3 C2 N1 109.7(3) . . ? C3 C2 H2 125.2 . . ? N1 C2 H2 125.2 . . ? C2 C3 N2 106.7(3) . . ? C2 C3 H3 126.7 . . ? N2 C3 H3 126.7 . . ? N2 C4 C5 112.7(3) . . ? N2 C4 H4A 109.0 . . ? C5 C4 H4A 109.0 . . ? N2 C4 H4B 109.0 . . ? C5 C4 H4B 109.0 . . ? H4A C4 H4B 107.8 . . ? O5 C5 C4 109.8(3) . . ? O5 C5 H5A 109.7 . . ? C4 C5 H5A 109.7 . . ? O5 C5 H5B 109.7 . . ? C4 C5 H5B 109.7 . . ? H5A C5 H5B 108.2 . . ? O5 C6 C7 108.4(3) . . ? O5 C6 H6A 110.0 . . ? C7 C6 H6A 110.0 . . ? O5 C6 H6B 110.0 . . ? C7 C6 H6B 110.0 . . ? H6A C6 H6B 108.4 . . ? C6 C7 N3 114.4(4) . . ? C6 C7 H7A 108.7 . . ? N3 C7 H7A 108.7 . . ? C6 C7 H7B 108.7 . . ? N3 C7 H7B 108.7 . . ? H7A C7 H7B 107.6 . . ? C9 C8 N3 106.7(3) . . ? C9 C8 H8 126.7 . . ? N3 C8 H8 126.7 . . ? C8 C9 N4 109.4(3) . . ? C8 C9 H9 125.3 . . ? N4 C9 H9 125.3 . . ? N4 C10 N3 111.2(3) . . ? N4 C10 H10 124.4 . . ? N3 C10 H10 124.4 . . ? O2 C11 O1 124.4(3) . . ? O2 C11 C12 120.9(2) . . ? O1 C11 C12 114.7(2) . . ? C13 C12 C17 119.4(2) . . ? C13 C12 C11 120.43(19) . . ? C17 C12 C11 120.0(2) . . ? C12 C13 C14 120.4(2) . . ? C12 C13 H13 119.8 . . ? C14 C13 H13 119.8 . . ? C15 C14 C13 120.3(3) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C14 C15 C16 119.7(2) . . ? C14 C15 H15 120.1 . . ? C16 C15 H15 120.1 . . ? C15 C16 C17 120.1(2) . . ? C15 C16 C18 119.4(2) . . ? C17 C16 C18 120.5(2) . . ? C16 C17 C12 120.0(2) . . ? C16 C17 H17 120.0 . . ? C12 C17 H17 120.0 . . ? O3 C18 O4 124.2(2) . . ? O3 C18 C16 119.4(2) . . ? O4 C18 C16 116.4(2) . . ? C1 N1 C2 105.5(3) . . ? C1 N1 Zn1 127.75(18) . . ? C2 N1 Zn1 126.5(2) . . ? C1 N2 C3 106.9(3) . . ? C1 N2 C4 125.4(3) . . ? C3 N2 C4 127.3(3) . . ? C10 N3 C8 106.9(3) . . ? C10 N3 C7 125.2(3) . . ? C8 N3 C7 127.8(3) . . ? C10 N4 C9 105.8(2) . . ? C10 N4 Zn1 128.46(19) . 3_445 ? C9 N4 Zn1 125.48(19) . 3_445 ? C11 O1 Zn1 114.02(17) . . ? C18 O4 Zn1 115.66(15) . 1_565 ? C6 O5 C5 112.3(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C2 C3 N2 1.1(4) . . . . ? N2 C4 C5 O5 -66.6(4) . . . . ? O5 C6 C7 N3 65.1(5) . . . . ? N3 C8 C9 N4 1.3(4) . . . . ? O2 C11 C12 C13 -173.7(2) . . . . ? O1 C11 C12 C13 3.4(3) . . . . ? O2 C11 C12 C17 1.3(4) . . . . ? O1 C11 C12 C17 178.3(2) . . . . ? C17 C12 C13 C14 -2.1(4) . . . . ? C11 C12 C13 C14 172.9(2) . . . . ? C12 C13 C14 C15 -1.5(4) . . . . ? C13 C14 C15 C16 3.0(4) . . . . ? C14 C15 C16 C17 -0.9(4) . . . . ? C14 C15 C16 C18 -177.6(3) . . . . ? C15 C16 C17 C12 -2.8(4) . . . . ? C18 C16 C17 C12 174.0(2) . . . . ? C13 C12 C17 C16 4.2(3) . . . . ? C11 C12 C17 C16 -170.7(2) . . . . ? C15 C16 C18 O3 26.9(4) . . . . ? C17 C16 C18 O3 -149.8(3) . . . . ? C15 C16 C18 O4 -155.2(2) . . . . ? C17 C16 C18 O4 28.0(4) . . . . ? N2 C1 N1 C2 0.1(3) . . . . ? N2 C1 N1 Zn1 -174.1(2) . . . . ? C3 C2 N1 C1 -0.8(4) . . . . ? C3 C2 N1 Zn1 173.5(2) . . . . ? O1 Zn1 N1 C1 -87.0(2) . . . . ? O4 Zn1 N1 C1 143.9(2) 1_545 . . . ? N4 Zn1 N1 C1 41.9(2) 3 . . . ? O1 Zn1 N1 C2 99.9(2) . . . . ? O4 Zn1 N1 C2 -29.2(2) 1_545 . . . ? N4 Zn1 N1 C2 -131.2(2) 3 . . . ? N1 C1 N2 C3 0.5(4) . . . . ? N1 C1 N2 C4 173.4(3) . . . . ? C2 C3 N2 C1 -1.0(4) . . . . ? C2 C3 N2 C4 -173.7(3) . . . . ? C5 C4 N2 C1 -89.1(4) . . . . ? C5 C4 N2 C3 82.3(5) . . . . ? N4 C10 N3 C8 1.1(3) . . . . ? N4 C10 N3 C7 -176.4(3) . . . . ? C9 C8 N3 C10 -1.4(3) . . . . ? C9 C8 N3 C7 175.9(3) . . . . ? C6 C7 N3 C10 -85.6(5) . . . . ? C6 C7 N3 C8 97.5(5) . . . . ? N3 C10 N4 C9 -0.3(3) . . . . ? N3 C10 N4 Zn1 174.02(18) . . . 3_445 ? C8 C9 N4 C10 -0.7(3) . . . . ? C8 C9 N4 Zn1 -175.2(2) . . . 3_445 ? O2 C11 O1 Zn1 5.6(4) . . . . ? C12 C11 O1 Zn1 -171.39(16) . . . . ? O4 Zn1 O1 C11 -168.48(17) 1_545 . . . ? N1 Zn1 O1 C11 68.0(2) . . . . ? N4 Zn1 O1 C11 -60.1(2) 3 . . . ? O3 C18 O4 Zn1 1.5(3) . . . 1_565 ? C16 C18 O4 Zn1 -176.27(16) . . . 1_565 ? C7 C6 O5 C5 163.1(3) . . . . ? C4 C5 O5 C6 148.8(3) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.323 _refine_diff_density_min -0.157 _refine_diff_density_rms 0.049 #===END data_compound4 _database_code_depnum_ccdc_archive 'CCDC 665627' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H18 Cd N4 O5' _chemical_formula_sum 'C18 H18 Cd N4 O5' _chemical_formula_weight 482.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.5350(5) _cell_length_b 10.2740(6) _cell_length_c 10.8080(7) _cell_angle_alpha 98.5590(10) _cell_angle_beta 100.1220(10) _cell_angle_gamma 94.8860(10) _cell_volume 916.54(10) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3420 _cell_measurement_theta_min 1.9 _cell_measurement_theta_max 28.3 _exptl_crystal_description Block _exptl_crystal_colour Orange _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.749 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 484 _exptl_absorpt_coefficient_mu 1.231 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.288 _exptl_absorpt_correction_T_max 0.317 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area-detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5803 _diffrn_reflns_av_R_equivalents 0.0218 _diffrn_reflns_av_sigmaI/netI 0.0594 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 28.29 _reflns_number_total 4229 _reflns_number_gt 3420 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0207P)^2^+1.1445P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4229 _refine_ls_number_parameters 253 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0580 _refine_ls_R_factor_gt 0.0425 _refine_ls_wR_factor_ref 0.0810 _refine_ls_wR_factor_gt 0.0733 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.51093(3) 0.31854(3) 0.38108(3) 0.02883(9) Uani 1 1 d . . . C16 C 0.6145(5) -0.2284(4) 0.0469(4) 0.0340(9) Uani 1 1 d . . . H16 H 0.6317 -0.2438 -0.0364 0.041 Uiso 1 1 calc R . . C17 C 0.5999(5) -0.1018(4) 0.1038(4) 0.0314(9) Uani 1 1 d . . . H17 H 0.6112 -0.0314 0.0598 0.038 Uiso 1 1 calc R . . C12 C 0.5682(4) -0.0787(3) 0.2272(4) 0.0243(8) Uani 1 1 d . . . C13 C 0.5613(4) -0.1825(3) 0.2952(4) 0.0250(8) Uani 1 1 d . . . H13 H 0.5442 -0.1670 0.3786 0.030 Uiso 1 1 calc R . . C11 C 0.5394(4) 0.0593(4) 0.2832(4) 0.0289(9) Uani 1 1 d . . . C1 C 0.7794(5) 0.1983(4) 0.5667(4) 0.0330(9) Uani 1 1 d . . . H1 H 0.7168 0.1167 0.5473 0.040 Uiso 1 1 calc R . . C2 C 0.8631(5) 0.4010(4) 0.5711(4) 0.0399(10) Uani 1 1 d . . . H2 H 0.8692 0.4873 0.5542 0.048 Uiso 1 1 calc R . . C3 C 0.9755(5) 0.3529(4) 0.6492(4) 0.0417(11) Uani 1 1 d . . . H3 H 1.0708 0.3989 0.6967 0.050 Uiso 1 1 calc R . . C4 C 0.9995(5) 0.1302(4) 0.7198(5) 0.0463(12) Uani 1 1 d . . . H4A H 1.1110 0.1643 0.7525 0.056 Uiso 1 1 calc R . . H4B H 0.9963 0.0457 0.6651 0.056 Uiso 1 1 calc R . . C5 C 0.9188(6) 0.1099(5) 0.8287(5) 0.0554(13) Uani 1 1 d . . . H5A H 0.8048 0.0853 0.7978 0.066 Uiso 1 1 calc R . . H5B H 0.9618 0.0388 0.8689 0.066 Uiso 1 1 calc R . . C6 C 0.8226(5) 0.2408(6) 0.9910(5) 0.0574(14) Uani 1 1 d . . . H6A H 0.8001 0.1586 1.0220 0.069 Uiso 1 1 calc R . . H6B H 0.7252 0.2587 0.9382 0.069 Uiso 1 1 calc R . . N2 N 0.9220(4) 0.2227(3) 0.6453(3) 0.0349(8) Uani 1 1 d . . . N1 N 0.7387(4) 0.3048(3) 0.5201(3) 0.0325(8) Uani 1 1 d . . . O1 O 0.5907(3) 0.1543(2) 0.2332(3) 0.0387(7) Uani 1 1 d . . . O2 O 0.4663(3) 0.0723(2) 0.3736(3) 0.0345(6) Uani 1 1 d . . . O5 O 0.9449(4) 0.2285(3) 0.9181(3) 0.0527(8) Uani 1 1 d . . . C14 C 0.5797(4) -0.3097(3) 0.2395(4) 0.0244(8) Uani 1 1 d . . . C18 C 0.5743(5) -0.4239(4) 0.3126(4) 0.0295(9) Uani 1 1 d . . . C15 C 0.6033(5) -0.3325(4) 0.1139(4) 0.0309(9) Uani 1 1 d . . . H15 H 0.6116 -0.4181 0.0751 0.037 Uiso 1 1 calc R . . O4 O 0.5606(4) -0.5384(3) 0.2483(3) 0.0492(8) Uani 1 1 d . . . O3 O 0.5836(4) -0.4016(3) 0.4298(3) 0.0441(8) Uani 1 1 d . . . N3 N 1.0045(4) 0.3174(3) 1.1951(3) 0.0382(8) Uani 1 1 d . . . C8 C 0.9838(6) 0.2450(5) 1.2884(5) 0.0486(12) Uani 1 1 d . . . H8 H 0.8869 0.2106 1.3053 0.058 Uiso 1 1 calc R . . C7 C 0.8760(5) 0.3512(5) 1.1006(5) 0.0554(13) Uani 1 1 d . . . H7A H 0.9135 0.4298 1.0697 0.067 Uiso 1 1 calc R . . H7B H 0.7857 0.3712 1.1407 0.067 Uiso 1 1 calc R . . N4 N 1.2446(4) 0.2975(3) 1.2977(3) 0.0350(8) Uani 1 1 d . . . C10 C 1.1629(5) 0.3467(4) 1.2051(4) 0.0391(10) Uani 1 1 d . . . H10 H 1.2090 0.3961 1.1526 0.047 Uiso 1 1 calc R . . C9 C 1.1317(5) 0.2332(4) 1.3511(4) 0.0442(11) Uani 1 1 d . . . H9 H 1.1540 0.1886 1.4198 0.053 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.03355(16) 0.02336(15) 0.03031(16) 0.00586(11) 0.00496(12) 0.00733(11) C16 0.048(2) 0.033(2) 0.026(2) 0.0085(17) 0.0115(19) 0.0123(19) C17 0.038(2) 0.0255(19) 0.034(2) 0.0145(17) 0.0060(18) 0.0112(17) C12 0.0264(19) 0.0179(17) 0.029(2) 0.0070(15) 0.0021(16) 0.0053(15) C13 0.0264(19) 0.0205(18) 0.028(2) 0.0042(15) 0.0042(16) 0.0024(15) C11 0.028(2) 0.0218(19) 0.034(2) 0.0043(17) -0.0016(18) 0.0055(16) C1 0.032(2) 0.031(2) 0.033(2) 0.0079(18) -0.0002(18) -0.0005(17) C2 0.040(2) 0.027(2) 0.049(3) -0.002(2) 0.006(2) 0.0021(19) C3 0.035(2) 0.034(2) 0.046(3) -0.008(2) -0.001(2) -0.0002(19) C4 0.044(3) 0.041(3) 0.051(3) 0.007(2) -0.003(2) 0.015(2) C5 0.061(3) 0.054(3) 0.044(3) 0.013(2) -0.008(3) 0.000(3) C6 0.031(2) 0.091(4) 0.046(3) 0.010(3) -0.002(2) 0.006(3) N2 0.0330(18) 0.0339(18) 0.035(2) 0.0040(15) -0.0006(15) 0.0058(15) N1 0.0310(18) 0.0321(18) 0.0322(19) 0.0035(15) 0.0020(15) 0.0045(15) O1 0.0506(18) 0.0212(14) 0.0477(18) 0.0092(13) 0.0150(15) 0.0053(13) O2 0.0430(16) 0.0265(14) 0.0372(17) 0.0058(12) 0.0134(14) 0.0095(12) O5 0.0427(18) 0.066(2) 0.0426(19) -0.0004(17) 0.0039(15) -0.0064(16) C14 0.0248(18) 0.0208(17) 0.028(2) 0.0053(15) 0.0044(16) 0.0043(15) C18 0.032(2) 0.0241(19) 0.038(2) 0.0102(17) 0.0124(18) 0.0095(16) C15 0.035(2) 0.0252(19) 0.032(2) 0.0007(17) 0.0056(18) 0.0088(17) O4 0.083(2) 0.0171(14) 0.050(2) 0.0076(13) 0.0183(18) 0.0067(14) O3 0.062(2) 0.0409(17) 0.0380(18) 0.0173(14) 0.0185(16) 0.0171(15) N3 0.0312(19) 0.047(2) 0.036(2) 0.0027(17) 0.0066(16) 0.0074(16) C8 0.041(3) 0.055(3) 0.051(3) 0.011(2) 0.013(2) -0.002(2) C7 0.036(3) 0.075(4) 0.056(3) 0.007(3) 0.006(2) 0.021(3) N4 0.0346(19) 0.0369(19) 0.034(2) 0.0056(16) 0.0065(16) 0.0068(16) C10 0.036(2) 0.047(3) 0.038(2) 0.007(2) 0.012(2) 0.010(2) C9 0.050(3) 0.041(3) 0.042(3) 0.010(2) 0.009(2) -0.001(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O4 2.266(3) 1_565 ? Cd1 N1 2.267(3) . ? Cd1 N4 2.272(3) 1_454 ? Cd1 O1 2.375(3) . ? Cd1 O3 2.395(3) 2_656 ? Cd1 O2 2.513(3) . ? C16 C17 1.380(5) . ? C16 C15 1.384(5) . ? C16 H16 0.9300 . ? C17 C12 1.397(5) . ? C17 H17 0.9300 . ? C12 C13 1.386(5) . ? C12 C11 1.514(5) . ? C13 C14 1.389(5) . ? C13 H13 0.9300 . ? C11 O2 1.246(5) . ? C11 O1 1.267(4) . ? C1 N1 1.318(5) . ? C1 N2 1.337(5) . ? C1 H1 0.9300 . ? C2 C3 1.341(6) . ? C2 N1 1.365(5) . ? C2 H2 0.9300 . ? C3 N2 1.368(5) . ? C3 H3 0.9300 . ? C4 N2 1.462(5) . ? C4 C5 1.495(6) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 O5 1.413(5) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 O5 1.417(5) . ? C6 C7 1.490(7) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C14 C15 1.396(5) . ? C14 C18 1.510(5) . ? C18 O3 1.241(5) . ? C18 O4 1.258(4) . ? C15 H15 0.9300 . ? O4 Cd1 2.266(3) 1_545 ? O3 Cd1 2.395(3) 2_656 ? N3 C10 1.342(5) . ? N3 C8 1.365(5) . ? N3 C7 1.464(5) . ? C8 C9 1.348(6) . ? C8 H8 0.9300 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? N4 C10 1.307(5) . ? N4 C9 1.378(5) . ? N4 Cd1 2.272(3) 1_656 ? C10 H10 0.9300 . ? C9 H9 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Cd1 N1 110.01(12) 1_565 . ? O4 Cd1 N4 90.57(12) 1_565 1_454 ? N1 Cd1 N4 158.60(12) . 1_454 ? O4 Cd1 O1 86.18(10) 1_565 . ? N1 Cd1 O1 88.33(11) . . ? N4 Cd1 O1 99.20(11) 1_454 . ? O4 Cd1 O3 118.30(10) 1_565 2_656 ? N1 Cd1 O3 83.66(11) . 2_656 ? N4 Cd1 O3 81.28(11) 1_454 2_656 ? O1 Cd1 O3 155.52(9) . 2_656 ? O4 Cd1 O2 138.08(10) 1_565 . ? N1 Cd1 O2 83.95(10) . . ? N4 Cd1 O2 84.41(10) 1_454 . ? O1 Cd1 O2 53.97(9) . . ? O3 Cd1 O2 102.05(9) 2_656 . ? C17 C16 C15 119.9(4) . . ? C17 C16 H16 120.1 . . ? C15 C16 H16 120.1 . . ? C16 C17 C12 120.3(3) . . ? C16 C17 H17 119.8 . . ? C12 C17 H17 119.8 . . ? C13 C12 C17 119.6(3) . . ? C13 C12 C11 121.3(3) . . ? C17 C12 C11 119.2(3) . . ? C12 C13 C14 120.3(3) . . ? C12 C13 H13 119.9 . . ? C14 C13 H13 119.9 . . ? O2 C11 O1 124.3(3) . . ? O2 C11 C12 118.6(3) . . ? O1 C11 C12 117.1(3) . . ? N1 C1 N2 111.4(3) . . ? N1 C1 H1 124.3 . . ? N2 C1 H1 124.3 . . ? C3 C2 N1 110.0(4) . . ? C3 C2 H2 125.0 . . ? N1 C2 H2 125.0 . . ? C2 C3 N2 106.4(4) . . ? C2 C3 H3 126.8 . . ? N2 C3 H3 126.8 . . ? N2 C4 C5 111.4(4) . . ? N2 C4 H4A 109.3 . . ? C5 C4 H4A 109.3 . . ? N2 C4 H4B 109.3 . . ? C5 C4 H4B 109.3 . . ? H4A C4 H4B 108.0 . . ? O5 C5 C4 109.1(4) . . ? O5 C5 H5A 109.9 . . ? C4 C5 H5A 109.9 . . ? O5 C5 H5B 109.9 . . ? C4 C5 H5B 109.9 . . ? H5A C5 H5B 108.3 . . ? O5 C6 C7 109.2(4) . . ? O5 C6 H6A 109.8 . . ? C7 C6 H6A 109.8 . . ? O5 C6 H6B 109.8 . . ? C7 C6 H6B 109.8 . . ? H6A C6 H6B 108.3 . . ? C1 N2 C3 106.8(3) . . ? C1 N2 C4 126.2(4) . . ? C3 N2 C4 126.8(4) . . ? C1 N1 C2 105.4(3) . . ? C1 N1 Cd1 126.1(3) . . ? C2 N1 Cd1 128.5(3) . . ? C11 O1 Cd1 93.7(2) . . ? C11 O2 Cd1 87.9(2) . . ? C5 O5 C6 112.7(4) . . ? C13 C14 C15 119.5(3) . . ? C13 C14 C18 121.1(3) . . ? C15 C14 C18 119.4(3) . . ? O3 C18 O4 123.8(4) . . ? O3 C18 C14 119.7(3) . . ? O4 C18 C14 116.5(3) . . ? C16 C15 C14 120.3(3) . . ? C16 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? C18 O4 Cd1 106.3(3) . 1_545 ? C18 O3 Cd1 153.2(3) . 2_656 ? C10 N3 C8 106.9(4) . . ? C10 N3 C7 127.5(4) . . ? C8 N3 C7 125.5(4) . . ? C9 C8 N3 106.4(4) . . ? C9 C8 H8 126.8 . . ? N3 C8 H8 126.8 . . ? N3 C7 C6 111.6(4) . . ? N3 C7 H7A 109.3 . . ? C6 C7 H7A 109.3 . . ? N3 C7 H7B 109.3 . . ? C6 C7 H7B 109.3 . . ? H7A C7 H7B 108.0 . . ? C10 N4 C9 105.4(4) . . ? C10 N4 Cd1 132.0(3) . 1_656 ? C9 N4 Cd1 122.4(3) . 1_656 ? N4 C10 N3 111.8(4) . . ? N4 C10 H10 124.1 . . ? N3 C10 H10 124.1 . . ? C8 C9 N4 109.5(4) . . ? C8 C9 H9 125.2 . . ? N4 C9 H9 125.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C15 C16 C17 C12 -2.3(6) . . . . ? C16 C17 C12 C13 4.0(6) . . . . ? C16 C17 C12 C11 -175.1(3) . . . . ? C17 C12 C13 C14 -2.4(5) . . . . ? C11 C12 C13 C14 176.6(3) . . . . ? C13 C12 C11 O2 -20.1(5) . . . . ? C17 C12 C11 O2 158.9(4) . . . . ? C13 C12 C11 O1 160.6(3) . . . . ? C17 C12 C11 O1 -20.3(5) . . . . ? N1 C2 C3 N2 1.2(5) . . . . ? N2 C4 C5 O5 -67.9(5) . . . . ? N1 C1 N2 C3 0.1(5) . . . . ? N1 C1 N2 C4 175.9(4) . . . . ? C2 C3 N2 C1 -0.8(5) . . . . ? C2 C3 N2 C4 -176.6(4) . . . . ? C5 C4 N2 C1 -72.4(5) . . . . ? C5 C4 N2 C3 102.5(5) . . . . ? N2 C1 N1 C2 0.7(5) . . . . ? N2 C1 N1 Cd1 179.4(3) . . . . ? C3 C2 N1 C1 -1.2(5) . . . . ? C3 C2 N1 Cd1 -179.8(3) . . . . ? O4 Cd1 N1 C1 -145.9(3) 1_565 . . . ? N4 Cd1 N1 C1 50.7(5) 1_454 . . . ? O1 Cd1 N1 C1 -60.6(3) . . . . ? O3 Cd1 N1 C1 96.2(3) 2_656 . . . ? O2 Cd1 N1 C1 -6.7(3) . . . . ? O4 Cd1 N1 C2 32.5(4) 1_565 . . . ? N4 Cd1 N1 C2 -130.9(4) 1_454 . . . ? O1 Cd1 N1 C2 117.8(3) . . . . ? O3 Cd1 N1 C2 -85.4(3) 2_656 . . . ? O2 Cd1 N1 C2 171.8(3) . . . . ? O2 C11 O1 Cd1 3.9(4) . . . . ? C12 C11 O1 Cd1 -176.9(3) . . . . ? O4 Cd1 O1 C11 -168.1(2) 1_565 . . . ? N1 Cd1 O1 C11 81.8(2) . . . . ? N4 Cd1 O1 C11 -78.1(2) 1_454 . . . ? O3 Cd1 O1 C11 11.1(4) 2_656 . . . ? O2 Cd1 O1 C11 -2.0(2) . . . . ? O1 C11 O2 Cd1 -3.7(4) . . . . ? C12 C11 O2 Cd1 177.1(3) . . . . ? O4 Cd1 O2 C11 23.1(3) 1_565 . . . ? N1 Cd1 O2 C11 -90.3(2) . . . . ? N4 Cd1 O2 C11 107.7(2) 1_454 . . . ? O1 Cd1 O2 C11 2.0(2) . . . . ? O3 Cd1 O2 C11 -172.5(2) 2_656 . . . ? C4 C5 O5 C6 153.6(4) . . . . ? C7 C6 O5 C5 167.5(4) . . . . ? C12 C13 C14 C15 -0.8(5) . . . . ? C12 C13 C14 C18 179.4(3) . . . . ? C13 C14 C18 O3 -13.6(6) . . . . ? C15 C14 C18 O3 166.5(4) . . . . ? C13 C14 C18 O4 166.6(4) . . . . ? C15 C14 C18 O4 -13.3(5) . . . . ? C17 C16 C15 C14 -0.9(6) . . . . ? C13 C14 C15 C16 2.5(6) . . . . ? C18 C14 C15 C16 -177.7(3) . . . . ? O3 C18 O4 Cd1 10.3(5) . . . 1_545 ? C14 C18 O4 Cd1 -169.9(2) . . . 1_545 ? O4 C18 O3 Cd1 -117.2(6) . . . 2_656 ? C14 C18 O3 Cd1 63.0(7) . . . 2_656 ? C10 N3 C8 C9 -0.2(5) . . . . ? C7 N3 C8 C9 177.9(4) . . . . ? C10 N3 C7 C6 95.2(6) . . . . ? C8 N3 C7 C6 -82.5(6) . . . . ? O5 C6 C7 N3 -70.1(5) . . . . ? C9 N4 C10 N3 -0.4(5) . . . . ? Cd1 N4 C10 N3 -174.5(3) 1_656 . . . ? C8 N3 C10 N4 0.4(5) . . . . ? C7 N3 C10 N4 -177.7(4) . . . . ? N3 C8 C9 N4 -0.1(5) . . . . ? C10 N4 C9 C8 0.3(5) . . . . ? Cd1 N4 C9 C8 175.1(3) 1_656 . . . ? _diffrn_measured_fraction_theta_max 0.925 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.593 _refine_diff_density_min -0.610 _refine_diff_density_rms 0.112 #===END data_compound5 _database_code_depnum_ccdc_archive 'CCDC 665628' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H18 Cd N4 O6' _chemical_formula_sum 'C18 H18 Cd N4 O6' _chemical_formula_weight 498.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.501(6) _cell_length_b 10.324(6) _cell_length_c 11.544(5) _cell_angle_alpha 82.720(19) _cell_angle_beta 71.95(2) _cell_angle_gamma 78.96(2) _cell_volume 943.0(9) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4028 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.490 _exptl_crystal_size_mid 0.477 _exptl_crystal_size_min 0.055 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.757 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 500 _exptl_absorpt_coefficient_mu 1.203 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8977 _exptl_absorpt_correction_T_max 1.1170 _exptl_absorpt_process_details ; Higashi,T (1995) Program for absorption correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9308 _diffrn_reflns_av_R_equivalents 0.0199 _diffrn_reflns_av_sigmaI/netI 0.0245 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4269 _reflns_number_gt 4028 _reflns_threshold_expression >2sigma(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction PROCESS-AUTO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0492P)^2^+0.2016P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4269 _refine_ls_number_parameters 266 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0242 _refine_ls_R_factor_gt 0.0215 _refine_ls_wR_factor_ref 0.0814 _refine_ls_wR_factor_gt 0.0710 _refine_ls_goodness_of_fit_ref 1.243 _refine_ls_restrained_S_all 1.243 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.47585(2) 0.805517(14) 0.615866(13) 0.02380(8) Uani 1 1 d . . . C1 C 0.7882(3) 0.6199(3) 0.4387(2) 0.0314(5) Uani 1 1 d . . . H1 H 0.7253 0.5519 0.4532 0.038 Uiso 1 1 calc R . . C2 C 0.8632(4) 0.8068(3) 0.4401(3) 0.0474(7) Uani 1 1 d . . . H2 H 0.8603 0.8930 0.4572 0.057 Uiso 1 1 calc R . . C3 C 0.9959(4) 0.7316(4) 0.3683(4) 0.0516(8) Uani 1 1 d . . . H3 H 1.0998 0.7560 0.3266 0.062 Uiso 1 1 calc R . . C4 C 1.0480(4) 0.5033(3) 0.2959(3) 0.0511(8) Uani 1 1 d . . . H4A H 1.0233 0.4203 0.3414 0.061 Uiso 1 1 calc R . . H4B H 1.1659 0.5057 0.2826 0.061 Uiso 1 1 calc R . . C5 C 1.0163(5) 0.5078(4) 0.1749(3) 0.0613(10) Uani 1 1 d . . . H5A H 1.0912 0.4364 0.1289 0.074 Uiso 1 1 calc R . . H5B H 0.9022 0.4940 0.1880 0.074 Uiso 1 1 calc R . . C6 C 0.8863(4) 0.7101(4) 0.1059(3) 0.0598(9) Uani 1 1 d . . . H6A H 0.8141 0.7183 0.1891 0.072 Uiso 1 1 calc R . . H6B H 0.8300 0.6705 0.0614 0.072 Uiso 1 1 calc R . . C7 C 0.9187(5) 0.8434(4) 0.0471(4) 0.0640(10) Uani 1 1 d . . . H7A H 0.8129 0.9034 0.0617 0.077 Uiso 1 1 calc R . . H7B H 0.9883 0.8763 0.0855 0.077 Uiso 1 1 calc R . . C8 C 0.9287(4) 0.8580(4) -0.1782(4) 0.0559(9) Uani 1 1 d . . . H8 H 0.8149 0.8670 -0.1702 0.067 Uiso 1 1 calc R . . C9 C 1.0557(4) 0.8556(3) -0.2831(3) 0.0497(7) Uani 1 1 d . . . H9 H 1.0430 0.8645 -0.3611 0.060 Uiso 1 1 calc R . . C10 C 1.1674(4) 0.8314(3) -0.1389(3) 0.0463(7) Uani 1 1 d . . . H10 H 1.2462 0.8190 -0.0962 0.056 Uiso 1 1 calc R . . C11 C 0.4190(3) 0.9314(2) 0.3529(2) 0.0262(5) Uani 1 1 d . . . C12 C 0.4435(3) 0.8234(2) 0.2688(2) 0.0233(4) Uani 1 1 d . . . C13 C 0.4619(3) 0.8584(2) 0.1456(2) 0.0261(5) Uani 1 1 d . . . H13 H 0.4557 0.9470 0.1166 0.031 Uiso 1 1 calc R . . C14 C 0.4896(3) 0.7606(2) 0.0659(2) 0.0280(5) Uani 1 1 d . . . C15 C 0.4997(3) 0.6284(2) 0.1097(2) 0.0289(5) Uani 1 1 d D . . H15 H 0.533(4) 0.571(3) 0.053(2) 0.035 Uiso 1 1 d D . . C16 C 0.4851(3) 0.5938(2) 0.2320(2) 0.0231(4) Uani 1 1 d . . . C17 C 0.4549(3) 0.6913(2) 0.31288(19) 0.0218(4) Uani 1 1 d . . . H17 H 0.4425 0.6683 0.3954 0.026 Uiso 1 1 calc R . . C18 C 0.5046(3) 0.4503(2) 0.2776(2) 0.0241(4) Uani 1 1 d . . . N1 N 0.7325(3) 0.7363(2) 0.4841(2) 0.0332(5) Uani 1 1 d . . . N2 N 0.9479(3) 0.6124(2) 0.3688(2) 0.0375(5) Uani 1 1 d . . . N3 N 1.0015(3) 0.8445(3) -0.0855(3) 0.0491(7) Uani 1 1 d . . . N4 N 1.2057(3) 0.8382(2) -0.2580(2) 0.0394(5) Uani 1 1 d . . . O1 O 0.3675(3) 0.90610(18) 0.46552(16) 0.0347(4) Uani 1 1 d . . . O2 O 0.4509(3) 1.04185(18) 0.30128(18) 0.0453(5) Uani 1 1 d . . . O3 O 0.4707(2) 0.36767(17) 0.22079(17) 0.0315(4) Uani 1 1 d . . . O4 O 0.5521(2) 0.41949(16) 0.37137(16) 0.0309(4) Uani 1 1 d . . . O5 O 0.5123(3) 0.8007(2) -0.05412(17) 0.0420(5) Uani 1 1 d . . . H5 H 0.5265 0.7362 -0.0931 0.063 Uiso 1 1 calc R . . O6 O 1.0401(3) 0.6289(3) 0.1062(2) 0.0566(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.03556(12) 0.01474(10) 0.01902(10) -0.00126(7) -0.00447(7) -0.00496(7) C1 0.0341(12) 0.0284(12) 0.0289(12) -0.0060(10) -0.0032(10) -0.0060(9) C2 0.0417(16) 0.0446(16) 0.0544(18) -0.0153(14) -0.0015(13) -0.0169(13) C3 0.0366(15) 0.0506(18) 0.066(2) -0.0150(16) -0.0023(14) -0.0178(13) C4 0.0457(17) 0.0438(17) 0.0512(18) -0.0117(15) -0.0010(14) 0.0064(13) C5 0.073(2) 0.056(2) 0.0473(19) -0.0195(17) -0.0027(17) -0.0060(18) C6 0.0443(18) 0.072(2) 0.0472(18) -0.0015(17) 0.0072(14) -0.0075(16) C7 0.057(2) 0.058(2) 0.054(2) -0.0100(18) 0.0168(17) -0.0031(17) C8 0.0360(16) 0.0450(18) 0.079(3) 0.0070(17) -0.0110(16) -0.0056(13) C9 0.0446(16) 0.0493(18) 0.0542(18) 0.0065(15) -0.0184(14) -0.0054(13) C10 0.0344(14) 0.0534(18) 0.0402(15) -0.0028(14) -0.0011(12) 0.0022(12) C11 0.0390(12) 0.0190(10) 0.0228(10) -0.0027(9) -0.0132(9) -0.0022(9) C12 0.0279(11) 0.0211(10) 0.0226(10) -0.0023(9) -0.0088(8) -0.0051(8) C13 0.0402(13) 0.0150(10) 0.0267(11) 0.0021(9) -0.0145(10) -0.0076(9) C14 0.0436(13) 0.0237(11) 0.0213(11) 0.0012(9) -0.0137(10) -0.0112(9) C15 0.0452(14) 0.0219(11) 0.0238(11) -0.0047(9) -0.0127(10) -0.0095(10) C16 0.0327(11) 0.0143(9) 0.0250(10) -0.0010(8) -0.0098(9) -0.0083(8) C17 0.0301(11) 0.0168(9) 0.0195(10) -0.0001(8) -0.0069(8) -0.0071(8) C18 0.0289(11) 0.0173(10) 0.0238(10) -0.0013(8) -0.0038(8) -0.0051(8) N1 0.0352(11) 0.0310(11) 0.0321(11) -0.0066(9) -0.0051(9) -0.0069(9) N2 0.0321(11) 0.0389(12) 0.0371(12) -0.0101(10) -0.0043(9) -0.0004(9) N3 0.0362(13) 0.0442(15) 0.0498(15) 0.0027(12) 0.0054(11) 0.0004(10) N4 0.0374(12) 0.0370(13) 0.0374(12) 0.0017(10) -0.0054(10) -0.0030(9) O1 0.0534(11) 0.0262(9) 0.0212(8) -0.0024(7) -0.0103(8) 0.0011(8) O2 0.0907(17) 0.0212(9) 0.0305(9) -0.0014(8) -0.0189(10) -0.0227(10) O3 0.0479(10) 0.0189(8) 0.0311(9) -0.0035(7) -0.0137(8) -0.0085(7) O4 0.0489(11) 0.0189(8) 0.0269(8) 0.0015(7) -0.0141(8) -0.0078(7) O5 0.0826(16) 0.0274(10) 0.0222(9) 0.0025(8) -0.0219(10) -0.0158(10) O6 0.0475(13) 0.0633(15) 0.0440(12) -0.0073(11) 0.0055(10) -0.0021(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O2 2.216(2) 2_676 ? Cd1 O1 2.2600(19) . ? Cd1 N1 2.282(3) . ? Cd1 N4 2.294(3) 1_456 ? Cd1 O4 2.362(2) 2_666 ? Cd1 O3 2.515(2) 2_666 ? C1 N1 1.316(3) . ? C1 N2 1.341(4) . ? C1 H1 0.9300 . ? C2 C3 1.345(5) . ? C2 N1 1.374(4) . ? C2 H2 0.9300 . ? C3 N2 1.368(4) . ? C3 H3 0.9300 . ? C4 N2 1.459(4) . ? C4 C5 1.497(5) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 O6 1.406(5) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 O6 1.413(4) . ? C6 C7 1.491(5) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 N3 1.473(5) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.349(5) . ? C8 N3 1.374(5) . ? C8 H8 0.9300 . ? C9 N4 1.367(4) . ? C9 H9 0.9300 . ? C10 N4 1.307(4) . ? C10 N3 1.340(4) . ? C10 H10 0.9300 . ? C11 O1 1.247(3) . ? C11 O2 1.255(3) . ? C11 C12 1.513(3) . ? C12 C13 1.390(3) . ? C12 C17 1.390(3) . ? C13 C14 1.390(4) . ? C13 H13 0.9300 . ? C14 O5 1.359(3) . ? C14 C15 1.391(3) . ? C15 C16 1.385(3) . ? C15 H15 0.880(18) . ? C16 C17 1.393(3) . ? C16 C18 1.504(3) . ? C17 H17 0.9300 . ? C18 O4 1.254(3) . ? C18 O3 1.262(3) . ? N4 Cd1 2.294(3) 1_654 ? O2 Cd1 2.216(2) 2_676 ? O3 Cd1 2.515(2) 2_666 ? O4 Cd1 2.362(2) 2_666 ? O5 H5 0.8200 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Cd1 O1 108.39(8) 2_676 . ? O2 Cd1 N1 97.82(10) 2_676 . ? O1 Cd1 N1 93.72(9) . . ? O2 Cd1 N4 92.57(10) 2_676 1_456 ? O1 Cd1 N4 86.01(9) . 1_456 ? N1 Cd1 N4 169.13(9) . 1_456 ? O2 Cd1 O4 145.43(7) 2_676 2_666 ? O1 Cd1 O4 105.99(7) . 2_666 ? N1 Cd1 O4 83.32(8) . 2_666 ? N4 Cd1 O4 86.30(9) 1_456 2_666 ? O2 Cd1 O3 91.53(7) 2_676 2_666 ? O1 Cd1 O3 158.37(7) . 2_666 ? N1 Cd1 O3 91.74(8) . 2_666 ? N4 Cd1 O3 84.75(8) 1_456 2_666 ? O4 Cd1 O3 53.93(6) 2_666 2_666 ? N1 C1 N2 110.9(2) . . ? N1 C1 H1 124.6 . . ? N2 C1 H1 124.6 . . ? C3 C2 N1 109.4(3) . . ? C3 C2 H2 125.3 . . ? N1 C2 H2 125.3 . . ? C2 C3 N2 106.4(3) . . ? C2 C3 H3 126.8 . . ? N2 C3 H3 126.8 . . ? N2 C4 C5 113.0(3) . . ? N2 C4 H4A 109.0 . . ? C5 C4 H4A 109.0 . . ? N2 C4 H4B 109.0 . . ? C5 C4 H4B 109.0 . . ? H4A C4 H4B 107.8 . . ? O6 C5 C4 112.4(3) . . ? O6 C5 H5A 109.1 . . ? C4 C5 H5A 109.1 . . ? O6 C5 H5B 109.1 . . ? C4 C5 H5B 109.1 . . ? H5A C5 H5B 107.9 . . ? O6 C6 C7 109.3(3) . . ? O6 C6 H6A 109.8 . . ? C7 C6 H6A 109.8 . . ? O6 C6 H6B 109.8 . . ? C7 C6 H6B 109.8 . . ? H6A C6 H6B 108.3 . . ? N3 C7 C6 113.9(3) . . ? N3 C7 H7A 108.8 . . ? C6 C7 H7A 108.8 . . ? N3 C7 H7B 108.8 . . ? C6 C7 H7B 108.8 . . ? H7A C7 H7B 107.7 . . ? C9 C8 N3 106.1(3) . . ? C9 C8 H8 127.0 . . ? N3 C8 H8 127.0 . . ? C8 C9 N4 110.0(3) . . ? C8 C9 H9 125.0 . . ? N4 C9 H9 125.0 . . ? N4 C10 N3 112.2(3) . . ? N4 C10 H10 123.9 . . ? N3 C10 H10 123.9 . . ? O1 C11 O2 125.2(2) . . ? O1 C11 C12 119.0(2) . . ? O2 C11 C12 115.7(2) . . ? C13 C12 C17 120.6(2) . . ? C13 C12 C11 118.7(2) . . ? C17 C12 C11 120.6(2) . . ? C12 C13 C14 119.7(2) . . ? C12 C13 H13 120.1 . . ? C14 C13 H13 120.1 . . ? O5 C14 C13 117.0(2) . . ? O5 C14 C15 123.1(2) . . ? C13 C14 C15 119.9(2) . . ? C16 C15 C14 120.1(2) . . ? C16 C15 H15 124(2) . . ? C14 C15 H15 115(2) . . ? C15 C16 C17 120.3(2) . . ? C15 C16 C18 119.9(2) . . ? C17 C16 C18 119.8(2) . . ? C12 C17 C16 119.2(2) . . ? C12 C17 H17 120.4 . . ? C16 C17 H17 120.4 . . ? O4 C18 O3 123.4(2) . . ? O4 C18 C16 117.9(2) . . ? O3 C18 C16 118.7(2) . . ? C1 N1 C2 106.0(2) . . ? C1 N1 Cd1 127.43(19) . . ? C2 N1 Cd1 126.5(2) . . ? C1 N2 C3 107.3(2) . . ? C1 N2 C4 126.8(3) . . ? C3 N2 C4 125.5(3) . . ? C10 N3 C8 106.4(3) . . ? C10 N3 C7 125.4(3) . . ? C8 N3 C7 128.2(3) . . ? C10 N4 C9 105.3(3) . . ? C10 N4 Cd1 123.5(2) . 1_654 ? C9 N4 Cd1 131.0(2) . 1_654 ? C11 O1 Cd1 137.30(18) . . ? C11 O2 Cd1 125.05(16) . 2_676 ? C18 O3 Cd1 87.62(14) . 2_666 ? C18 O4 Cd1 94.90(14) . 2_666 ? C14 O5 H5 109.5 . . ? C5 O6 C6 111.9(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C2 C3 N2 -0.7(4) . . . . ? N2 C4 C5 O6 55.2(4) . . . . ? O6 C6 C7 N3 69.9(5) . . . . ? N3 C8 C9 N4 1.3(4) . . . . ? O1 C11 C12 C13 164.9(2) . . . . ? O2 C11 C12 C13 -13.9(3) . . . . ? O1 C11 C12 C17 -17.9(4) . . . . ? O2 C11 C12 C17 163.2(2) . . . . ? C17 C12 C13 C14 0.9(4) . . . . ? C11 C12 C13 C14 178.0(2) . . . . ? C12 C13 C14 O5 -177.8(2) . . . . ? C12 C13 C14 C15 -0.4(4) . . . . ? O5 C14 C15 C16 176.2(3) . . . . ? C13 C14 C15 C16 -1.1(4) . . . . ? C14 C15 C16 C17 2.0(4) . . . . ? C14 C15 C16 C18 -177.0(2) . . . . ? C13 C12 C17 C16 0.0(3) . . . . ? C11 C12 C17 C16 -177.1(2) . . . . ? C15 C16 C17 C12 -1.4(3) . . . . ? C18 C16 C17 C12 177.5(2) . . . . ? C15 C16 C18 O4 154.1(2) . . . . ? C17 C16 C18 O4 -24.8(3) . . . . ? C15 C16 C18 O3 -26.7(3) . . . . ? C17 C16 C18 O3 154.3(2) . . . . ? N2 C1 N1 C2 0.4(3) . . . . ? N2 C1 N1 Cd1 -177.07(17) . . . . ? C3 C2 N1 C1 0.2(4) . . . . ? C3 C2 N1 Cd1 177.7(2) . . . . ? O2 Cd1 N1 C1 154.5(2) 2_676 . . . ? O1 Cd1 N1 C1 -96.4(2) . . . . ? N4 Cd1 N1 C1 -8.2(6) 1_456 . . . ? O4 Cd1 N1 C1 9.3(2) 2_666 . . . ? O3 Cd1 N1 C1 62.7(2) 2_666 . . . ? O2 Cd1 N1 C2 -22.5(3) 2_676 . . . ? O1 Cd1 N1 C2 86.6(3) . . . . ? N4 Cd1 N1 C2 174.8(4) 1_456 . . . ? O4 Cd1 N1 C2 -167.7(3) 2_666 . . . ? O3 Cd1 N1 C2 -114.3(3) 2_666 . . . ? N1 C1 N2 C3 -0.9(3) . . . . ? N1 C1 N2 C4 -175.0(3) . . . . ? C2 C3 N2 C1 0.9(4) . . . . ? C2 C3 N2 C4 175.2(3) . . . . ? C5 C4 N2 C1 81.9(4) . . . . ? C5 C4 N2 C3 -91.2(4) . . . . ? N4 C10 N3 C8 1.3(4) . . . . ? N4 C10 N3 C7 -179.0(3) . . . . ? C9 C8 N3 C10 -1.5(4) . . . . ? C9 C8 N3 C7 178.8(3) . . . . ? C6 C7 N3 C10 -92.8(5) . . . . ? C6 C7 N3 C8 86.9(5) . . . . ? N3 C10 N4 C9 -0.5(4) . . . . ? N3 C10 N4 Cd1 -175.4(2) . . . 1_654 ? C8 C9 N4 C10 -0.5(4) . . . . ? C8 C9 N4 Cd1 173.9(2) . . . 1_654 ? O2 C11 O1 Cd1 -101.5(3) . . . . ? C12 C11 O1 Cd1 79.7(3) . . . . ? O2 Cd1 O1 C11 93.3(3) 2_676 . . . ? N1 Cd1 O1 C11 -6.2(3) . . . . ? N4 Cd1 O1 C11 -175.3(3) 1_456 . . . ? O4 Cd1 O1 C11 -90.3(3) 2_666 . . . ? O3 Cd1 O1 C11 -110.4(3) 2_666 . . . ? O1 C11 O2 Cd1 26.0(4) . . . 2_676 ? C12 C11 O2 Cd1 -155.18(17) . . . 2_676 ? O4 C18 O3 Cd1 3.6(2) . . . 2_666 ? C16 C18 O3 Cd1 -175.51(19) . . . 2_666 ? O3 C18 O4 Cd1 -3.8(3) . . . 2_666 ? C16 C18 O4 Cd1 175.28(18) . . . 2_666 ? C4 C5 O6 C6 -104.7(4) . . . . ? C7 C6 O6 C5 172.1(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O5 H5 O3 0.82 1.92 2.706(3) 160.0 2_665 _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.549 _refine_diff_density_min -0.750 _refine_diff_density_rms 0.167 #===END data_compound6 _database_code_depnum_ccdc_archive 'CCDC 665629' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H18 N4 O6 Zn' _chemical_formula_sum 'C18 H18 N4 O6 Zn' _chemical_formula_weight 451.73 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.5520(5) _cell_length_b 15.4790(7) _cell_length_c 12.7160(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.7030(10) _cell_angle_gamma 90.00 _cell_volume 1879.99(18) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4000 _cell_measurement_theta_min 2.1 _cell_measurement_theta_max 28.4 _exptl_crystal_description Block _exptl_crystal_colour Orange _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.596 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 928 _exptl_absorpt_coefficient_mu 1.351 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.217 _exptl_absorpt_correction_T_max 0.267 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area-detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11402 _diffrn_reflns_av_R_equivalents 0.0239 _diffrn_reflns_av_sigmaI/netI 0.0279 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 28.40 _reflns_number_total 4564 _reflns_number_gt 4000 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0726P)^2^+1.0870P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4564 _refine_ls_number_parameters 272 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0459 _refine_ls_R_factor_gt 0.0410 _refine_ls_wR_factor_ref 0.1195 _refine_ls_wR_factor_gt 0.1160 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.78436(2) 0.048968(17) 0.854601(18) 0.02791(11) Uani 1 1 d . . . C1 C 0.6901(3) -0.11977(18) 0.94237(19) 0.0410(6) Uani 1 1 d . . . H1 H 0.6453 -0.0917 0.9972 0.049 Uiso 1 1 calc R . . C2 C 0.8133(4) -0.14494(19) 0.8058(2) 0.0507(7) Uani 1 1 d . . . H2 H 0.8699 -0.1367 0.7477 0.061 Uiso 1 1 calc R . . C3 C 0.7635(4) -0.2212(2) 0.8382(3) 0.0614(9) Uani 1 1 d . . . H3 H 0.7795 -0.2749 0.8077 0.074 Uiso 1 1 calc R . . C4 C 0.5954(5) -0.2656(3) 0.9839(3) 0.0878(15) Uani 1 1 d . . . C5 C 0.6732(7) -0.3297(3) 1.0428(4) 0.0693(13) Uani 0.80 1 d P . . C5' C 0.598(2) -0.2819(15) 1.0677(14) 0.069(6) Uani 0.20 1 d P . . C6 C 0.8362(5) -0.3460(3) 1.1663(3) 0.0720(10) Uani 1 1 d . . . H6A H 0.9129 -0.3499 1.1172 0.086 Uiso 1 1 calc R . . H6B H 0.7920 -0.4022 1.1706 0.086 Uiso 1 1 calc R . . C7 C 0.8894(4) -0.3206(3) 1.2695(2) 0.0678(10) Uani 1 1 d . . . H7A H 0.9108 -0.2594 1.2679 0.081 Uiso 1 1 calc R . . H7B H 0.9763 -0.3512 1.2830 0.081 Uiso 1 1 calc R . . C8 C 0.6709(4) -0.2970(3) 1.3763(3) 0.0737(12) Uani 1 1 d . . . H8 H 0.6265 -0.2558 1.3344 0.088 Uiso 1 1 calc R . . C9 C 0.6252(4) -0.3292(3) 1.4683(3) 0.0732(12) Uani 1 1 d . . . H9 H 0.5421 -0.3136 1.5006 0.088 Uiso 1 1 calc R . . C10 C 0.8178(3) -0.39164(18) 1.43696(18) 0.0395(6) Uani 1 1 d . . . H10 H 0.8951 -0.4281 1.4421 0.047 Uiso 1 1 calc R . . C11 C 0.5190(2) 0.07230(15) 0.78464(17) 0.0279(4) Uani 1 1 d . . . C12 C 0.3966(2) 0.07558(14) 0.70904(16) 0.0262(4) Uani 1 1 d . . . C13 C 0.4196(2) 0.07532(15) 0.60103(17) 0.0287(4) Uani 1 1 d . . . H13 H 0.5101 0.0804 0.5756 0.034 Uiso 1 1 calc R . . C14 C 0.3065(2) 0.06735(15) 0.53107(17) 0.0300(4) Uani 1 1 d . . . C15 C 0.1716(2) 0.05998(15) 0.56913(17) 0.0284(4) Uani 1 1 d . . . H15 H 0.0966 0.0532 0.5226 0.034 Uiso 1 1 calc R . . C16 C 0.1484(2) 0.06273(14) 0.67702(17) 0.0269(4) Uani 1 1 d . . . C17 C 0.2605(2) 0.07124(15) 0.74711(17) 0.0279(4) Uani 1 1 d . . . H17 H 0.2448 0.0740 0.8191 0.033 Uiso 1 1 calc R . . C18 C 0.0012(2) 0.04946(15) 0.71495(18) 0.0311(5) Uani 1 1 d . . . N1 N 0.7676(2) -0.08074(15) 0.87176(16) 0.0358(4) Uani 1 1 d . . . N2 N 0.6840(3) -0.20433(16) 0.92532(18) 0.0521(6) Uani 1 1 d . . . N3 N 0.7947(2) -0.33691(17) 1.35699(15) 0.0419(5) Uani 1 1 d . . . N4 N 0.7188(2) -0.38769(14) 1.50689(15) 0.0342(4) Uani 1 1 d . . . O1 O 0.64081(16) 0.08726(12) 0.74895(13) 0.0334(4) Uani 1 1 d . . . O2 O 0.49901(19) 0.05189(14) 0.87770(14) 0.0439(5) Uani 1 1 d . . . O3 O -0.02743(17) 0.07943(14) 0.80548(14) 0.0408(4) Uani 1 1 d . . . O4 O -0.08260(19) 0.01012(17) 0.65789(15) 0.0515(5) Uani 1 1 d . . . O5 O 0.3336(2) 0.06491(14) 0.42587(13) 0.0437(5) Uani 1 1 d . . . H5 H 0.2600 0.0588 0.3929 0.080(14) Uiso 1 1 calc R . . O6 O 0.7382(3) -0.2843(2) 1.13061(19) 0.0771(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.02007(15) 0.03907(17) 0.02459(15) -0.00350(9) 0.00068(10) -0.00125(9) C1 0.0456(14) 0.0499(14) 0.0275(11) 0.0003(10) -0.0024(10) -0.0063(11) C2 0.0673(19) 0.0461(15) 0.0387(14) -0.0039(11) 0.0086(13) 0.0126(13) C3 0.093(3) 0.0389(15) 0.0518(17) -0.0072(12) -0.0109(17) 0.0082(15) C4 0.111(3) 0.081(3) 0.071(2) 0.040(2) -0.043(2) -0.055(2) C5 0.100(4) 0.046(2) 0.061(3) 0.0130(19) -0.018(3) 0.000(2) C5' 0.066(11) 0.088(14) 0.053(9) 0.033(10) -0.017(8) -0.048(11) C6 0.102(3) 0.072(2) 0.0419(16) 0.0054(16) 0.0035(18) -0.012(2) C7 0.0547(19) 0.112(3) 0.0362(15) 0.0272(17) 0.0045(13) -0.0033(19) C8 0.088(3) 0.081(2) 0.0518(18) 0.0303(18) 0.0101(17) 0.045(2) C9 0.071(2) 0.094(3) 0.0548(18) 0.0269(18) 0.0174(16) 0.051(2) C10 0.0330(12) 0.0563(15) 0.0294(11) 0.0137(10) 0.0017(9) 0.0089(11) C11 0.0213(10) 0.0350(10) 0.0274(10) -0.0032(8) -0.0004(8) -0.0013(8) C12 0.0211(10) 0.0313(10) 0.0261(10) -0.0007(8) -0.0005(8) -0.0009(8) C13 0.0197(10) 0.0402(11) 0.0263(10) 0.0005(8) 0.0030(8) -0.0001(8) C14 0.0258(11) 0.0412(12) 0.0231(10) 0.0002(8) 0.0013(8) 0.0018(8) C15 0.0205(10) 0.0385(11) 0.0262(10) -0.0004(8) -0.0014(8) 0.0007(8) C16 0.0185(10) 0.0359(11) 0.0263(10) -0.0019(8) 0.0016(8) 0.0013(7) C17 0.0215(10) 0.0382(11) 0.0240(9) -0.0034(8) 0.0014(8) 0.0005(8) C18 0.0194(10) 0.0461(13) 0.0279(10) -0.0006(9) 0.0015(8) -0.0017(8) N1 0.0377(11) 0.0395(11) 0.0302(9) -0.0011(8) 0.0016(8) 0.0026(8) N2 0.0735(17) 0.0471(13) 0.0353(11) 0.0086(10) -0.0170(11) -0.0165(12) N3 0.0407(12) 0.0559(14) 0.0291(10) 0.0134(9) -0.0009(9) 0.0005(9) N4 0.0317(10) 0.0435(11) 0.0273(9) 0.0076(8) -0.0002(7) 0.0064(8) O1 0.0191(7) 0.0502(10) 0.0310(8) 0.0050(7) -0.0005(6) -0.0038(6) O2 0.0283(9) 0.0790(14) 0.0244(8) 0.0038(8) -0.0008(7) -0.0086(8) O3 0.0222(8) 0.0654(12) 0.0350(9) -0.0122(8) 0.0078(6) -0.0051(8) O4 0.0270(9) 0.0911(16) 0.0366(10) -0.0138(10) 0.0024(7) -0.0180(9) O5 0.0292(9) 0.0799(14) 0.0221(8) -0.0016(8) 0.0026(7) -0.0029(8) O6 0.0823(18) 0.097(2) 0.0510(13) 0.0310(13) -0.0201(12) -0.0043(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O3 1.9678(17) 1_655 ? Zn1 O1 1.9978(16) . ? Zn1 N4 2.0164(19) 2_657 ? Zn1 N1 2.026(2) . ? C1 N1 1.317(3) . ? C1 N2 1.328(4) . ? C1 H1 0.9300 . ? C2 C3 1.339(5) . ? C2 N1 1.374(3) . ? C2 H2 0.9300 . ? C3 N2 1.376(4) . ? C3 H3 0.9300 . ? C4 C5' 1.094(16) . ? C4 C5 1.443(6) . ? C4 N2 1.479(4) . ? C5 C5' 1.08(3) . ? C5 O6 1.453(6) . ? C5' O6 1.553(18) . ? C6 O6 1.408(5) . ? C6 C7 1.455(5) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 N3 1.464(3) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.349(5) . ? C8 N3 1.359(4) . ? C8 H8 0.9300 . ? C9 N4 1.360(3) . ? C9 H9 0.9300 . ? C10 N4 1.308(3) . ? C10 N3 1.340(3) . ? C10 H10 0.9300 . ? C11 O2 1.242(3) . ? C11 O1 1.275(3) . ? C11 C12 1.506(3) . ? C12 C13 1.394(3) . ? C12 C17 1.394(3) . ? C13 C14 1.397(3) . ? C13 H13 0.9300 . ? C14 O5 1.366(3) . ? C14 C15 1.387(3) . ? C15 C16 1.393(3) . ? C15 H15 0.9300 . ? C16 C17 1.391(3) . ? C16 C18 1.506(3) . ? C17 H17 0.9300 . ? C18 O4 1.235(3) . ? C18 O3 1.274(3) . ? N4 Zn1 2.0164(19) 2_647 ? O3 Zn1 1.9678(17) 1_455 ? O5 H5 0.8200 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Zn1 O1 109.73(7) 1_655 . ? O3 Zn1 N4 100.62(8) 1_655 2_657 ? O1 Zn1 N4 115.19(8) . 2_657 ? O3 Zn1 N1 110.20(9) 1_655 . ? O1 Zn1 N1 108.18(8) . . ? N4 Zn1 N1 112.69(8) 2_657 . ? N1 C1 N2 111.4(3) . . ? N1 C1 H1 124.3 . . ? N2 C1 H1 124.3 . . ? C3 C2 N1 109.5(3) . . ? C3 C2 H2 125.2 . . ? N1 C2 H2 125.2 . . ? C2 C3 N2 106.3(3) . . ? C2 C3 H3 126.8 . . ? N2 C3 H3 126.8 . . ? C5' C4 C5 48.1(14) . . ? C5' C4 N2 129.2(9) . . ? C5 C4 N2 114.1(4) . . ? C5' C5 C4 48.8(9) . . ? C5' C5 O6 73.9(9) . . ? C4 C5 O6 106.1(4) . . ? C5 C5' C4 83.1(17) . . ? C5 C5' O6 64.0(11) . . ? C4 C5' O6 121.0(15) . . ? O6 C6 C7 109.3(3) . . ? O6 C6 H6A 109.8 . . ? C7 C6 H6A 109.8 . . ? O6 C6 H6B 109.8 . . ? C7 C6 H6B 109.8 . . ? H6A C6 H6B 108.3 . . ? C6 C7 N3 115.3(3) . . ? C6 C7 H7A 108.5 . . ? N3 C7 H7A 108.5 . . ? C6 C7 H7B 108.5 . . ? N3 C7 H7B 108.5 . . ? H7A C7 H7B 107.5 . . ? C9 C8 N3 106.3(3) . . ? C9 C8 H8 126.9 . . ? N3 C8 H8 126.9 . . ? C8 C9 N4 109.9(3) . . ? C8 C9 H9 125.0 . . ? N4 C9 H9 125.0 . . ? N4 C10 N3 111.9(2) . . ? N4 C10 H10 124.1 . . ? N3 C10 H10 124.1 . . ? O2 C11 O1 122.5(2) . . ? O2 C11 C12 119.29(19) . . ? O1 C11 C12 118.14(19) . . ? C13 C12 C17 120.1(2) . . ? C13 C12 C11 119.87(19) . . ? C17 C12 C11 119.80(19) . . ? C12 C13 C14 119.8(2) . . ? C12 C13 H13 120.1 . . ? C14 C13 H13 120.1 . . ? O5 C14 C15 121.8(2) . . ? O5 C14 C13 118.2(2) . . ? C15 C14 C13 120.0(2) . . ? C14 C15 C16 120.1(2) . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C17 C16 C15 120.2(2) . . ? C17 C16 C18 121.5(2) . . ? C15 C16 C18 118.13(19) . . ? C16 C17 C12 119.7(2) . . ? C16 C17 H17 120.1 . . ? C12 C17 H17 120.1 . . ? O4 C18 O3 124.4(2) . . ? O4 C18 C16 118.7(2) . . ? O3 C18 C16 116.8(2) . . ? C1 N1 C2 105.6(2) . . ? C1 N1 Zn1 125.00(19) . . ? C2 N1 Zn1 128.66(19) . . ? C1 N2 C3 107.2(2) . . ? C1 N2 C4 125.0(3) . . ? C3 N2 C4 127.5(3) . . ? C10 N3 C8 106.6(2) . . ? C10 N3 C7 126.0(2) . . ? C8 N3 C7 127.3(3) . . ? C10 N4 C9 105.3(2) . . ? C10 N4 Zn1 126.14(16) . 2_647 ? C9 N4 Zn1 128.48(19) . 2_647 ? C11 O1 Zn1 109.17(14) . . ? C18 O3 Zn1 114.01(15) . 1_455 ? C14 O5 H5 109.5 . . ? C6 O6 C5 101.2(3) . . ? C6 O6 C5' 138.4(9) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C2 C3 N2 0.6(4) . . . . ? N2 C4 C5 C5' 122.0(12) . . . . ? C5' C4 C5 O6 -50.5(11) . . . . ? N2 C4 C5 O6 71.5(5) . . . . ? O6 C5 C5' C4 129.5(9) . . . . ? C4 C5 C5' O6 -129.5(9) . . . . ? N2 C4 C5' C5 -88.6(17) . . . . ? C5 C4 C5' O6 54.1(17) . . . . ? N2 C4 C5' O6 -35(3) . . . . ? O6 C6 C7 N3 76.9(4) . . . . ? N3 C8 C9 N4 0.4(5) . . . . ? O2 C11 C12 C13 -162.9(2) . . . . ? O1 C11 C12 C13 14.2(3) . . . . ? O2 C11 C12 C17 11.6(3) . . . . ? O1 C11 C12 C17 -171.3(2) . . . . ? C17 C12 C13 C14 -2.5(4) . . . . ? C11 C12 C13 C14 171.9(2) . . . . ? C12 C13 C14 O5 -178.2(2) . . . . ? C12 C13 C14 C15 0.2(4) . . . . ? O5 C14 C15 C16 180.0(2) . . . . ? C13 C14 C15 C16 1.6(4) . . . . ? C14 C15 C16 C17 -1.2(3) . . . . ? C14 C15 C16 C18 -176.6(2) . . . . ? C15 C16 C17 C12 -1.1(3) . . . . ? C18 C16 C17 C12 174.2(2) . . . . ? C13 C12 C17 C16 2.9(3) . . . . ? C11 C12 C17 C16 -171.5(2) . . . . ? C17 C16 C18 O4 -152.1(3) . . . . ? C15 C16 C18 O4 23.2(3) . . . . ? C17 C16 C18 O3 27.2(3) . . . . ? C15 C16 C18 O3 -157.4(2) . . . . ? N2 C1 N1 C2 0.1(3) . . . . ? N2 C1 N1 Zn1 171.02(18) . . . . ? C3 C2 N1 C1 -0.4(3) . . . . ? C3 C2 N1 Zn1 -170.9(2) . . . . ? O3 Zn1 N1 C1 147.9(2) 1_655 . . . ? O1 Zn1 N1 C1 -92.1(2) . . . . ? N4 Zn1 N1 C1 36.4(2) 2_657 . . . ? O3 Zn1 N1 C2 -43.2(3) 1_655 . . . ? O1 Zn1 N1 C2 76.7(3) . . . . ? N4 Zn1 N1 C2 -154.8(2) 2_657 . . . ? N1 C1 N2 C3 0.3(3) . . . . ? N1 C1 N2 C4 -174.0(3) . . . . ? C2 C3 N2 C1 -0.6(4) . . . . ? C2 C3 N2 C4 173.5(3) . . . . ? C5' C4 N2 C1 -62(2) . . . . ? C5 C4 N2 C1 -116.8(5) . . . . ? C5' C4 N2 C3 125(2) . . . . ? C5 C4 N2 C3 70.1(5) . . . . ? N4 C10 N3 C8 -1.5(4) . . . . ? N4 C10 N3 C7 175.4(3) . . . . ? C9 C8 N3 C10 0.6(5) . . . . ? C9 C8 N3 C7 -176.3(4) . . . . ? C6 C7 N3 C10 115.5(4) . . . . ? C6 C7 N3 C8 -68.1(6) . . . . ? N3 C10 N4 C9 1.8(4) . . . . ? N3 C10 N4 Zn1 -175.07(18) . . . 2_647 ? C8 C9 N4 C10 -1.3(5) . . . . ? C8 C9 N4 Zn1 175.4(3) . . . 2_647 ? O2 C11 O1 Zn1 11.7(3) . . . . ? C12 C11 O1 Zn1 -165.35(16) . . . . ? O3 Zn1 O1 C11 -175.81(15) 1_655 . . . ? N4 Zn1 O1 C11 -63.16(17) 2_657 . . . ? N1 Zn1 O1 C11 63.94(17) . . . . ? O4 C18 O3 Zn1 5.2(3) . . . 1_455 ? C16 C18 O3 Zn1 -174.11(16) . . . 1_455 ? C7 C6 O6 C5 -166.6(4) . . . . ? C7 C6 O6 C5' -143.1(11) . . . . ? C5' C5 O6 C6 156.7(9) . . . . ? C4 C5 O6 C6 -166.2(4) . . . . ? C4 C5 O6 C5' 37.2(8) . . . . ? C5 C5' O6 C6 -35.8(14) . . . . ? C4 C5' O6 C6 -99.2(18) . . . . ? C4 C5' O6 C5 -63(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O5 H5 O4 0.82 2.10 2.858(3) 154.3 3_556 _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.979 _refine_diff_density_min -0.696 _refine_diff_density_rms 0.125 #===END data_compound7 _database_code_depnum_ccdc_archive 'CCDC 665630' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H41 N8 O13 Zn2' _chemical_formula_sum 'C36 H41 N8 O13 Zn2' _chemical_formula_weight 924.51 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 17.8830(15) _cell_length_b 11.1160(16) _cell_length_c 21.424(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.301(3) _cell_angle_gamma 90.00 _cell_volume 4202.8(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2145 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 28.3 _exptl_crystal_description Block _exptl_crystal_colour Orange _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.461 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1908 _exptl_absorpt_coefficient_mu 1.212 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.89 _exptl_absorpt_correction_T_max 0.95 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area-detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12760 _diffrn_reflns_av_R_equivalents 0.0646 _diffrn_reflns_av_sigmaI/netI 0.0942 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 28.28 _reflns_number_total 5052 _reflns_number_gt 2141 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0673P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0013(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5052 _refine_ls_number_parameters 237 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1678 _refine_ls_R_factor_gt 0.0749 _refine_ls_wR_factor_ref 0.2014 _refine_ls_wR_factor_gt 0.1698 _refine_ls_goodness_of_fit_ref 1.172 _refine_ls_restrained_S_all 1.250 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.08221(4) 0.07230(6) 0.61827(3) 0.0642(3) Uani 1 1 d . . . C1 C -0.0690(4) -0.0521(6) 0.5849(3) 0.0674(17) Uani 1 1 d . . . H1 H -0.0852 -0.0022 0.5505 0.081 Uiso 1 1 calc R . . C2 C -0.0030(4) -0.1289(7) 0.6669(3) 0.087(2) Uiso 1 1 d . . . H2 H 0.0352 -0.1429 0.7010 0.105 Uiso 1 1 calc R . . C3 C -0.0647(5) -0.1965(7) 0.6511(3) 0.096(2) Uani 1 1 d . . . H3 H -0.0768 -0.2656 0.6718 0.115 Uiso 1 1 calc R . . C4 C -0.1790(4) -0.1891(7) 0.5657(3) 0.097(2) Uani 1 1 d . . . H4A H -0.1746 -0.2736 0.5558 0.116 Uiso 1 1 calc R . . H4B H -0.1915 -0.1455 0.5262 0.116 Uiso 1 1 calc R . . C5 C -0.2409(5) -0.1728(8) 0.6038(4) 0.119(3) Uiso 1 1 d . . . H5A H -0.2879 -0.2053 0.5811 0.143 Uiso 1 1 calc R . . H5B H -0.2286 -0.2154 0.6437 0.143 Uiso 1 1 calc R . . C6 C -0.3062(6) -0.0279(9) 0.6516(5) 0.137(3) Uiso 1 1 d . . . H6A H -0.2998 -0.0787 0.6889 0.164 Uiso 1 1 calc R . . H6B H -0.3559 -0.0430 0.6272 0.164 Uiso 1 1 calc R . . C7 C -0.2986(5) 0.0968(8) 0.6694(4) 0.121(3) Uiso 1 1 d . . . H7A H -0.3408 0.1200 0.6901 0.145 Uiso 1 1 calc R . . H7B H -0.3005 0.1457 0.6317 0.145 Uiso 1 1 calc R . . C8' C -0.1812(11) 0.1922(16) 0.6994(7) 0.102(6) Uiso 0.50 1 d PD . . C8 C -0.1525(10) 0.1460(15) 0.6926(7) 0.089(5) Uiso 0.50 1 d PD . . C9 C -0.0955(10) 0.1387(15) 0.7446(7) 0.086(5) Uani 0.50 1 d P . . C9' C -0.1176(10) 0.1929(16) 0.7536(9) 0.092(7) Uiso 0.50 1 d PD . . C10 C -0.2077(4) 0.0840(6) 0.7729(3) 0.0788(19) Uani 1 1 d D . . H10 H -0.2412 0.0448 0.7951 0.095 Uiso 1 1 calc R . . C11 C 0.0217(3) 0.2904(6) 0.5828(3) 0.0671(17) Uani 1 1 d . . . C12 C 0.0096(3) 0.3996(5) 0.5399(3) 0.0602(15) Uani 1 1 d . . . C13 C -0.0048(3) 0.5116(6) 0.5634(3) 0.0688(16) Uani 1 1 d . . . H13 H -0.0078 0.5207 0.6061 0.083 Uiso 1 1 calc R . . C14 C 0.0147(3) 0.3900(6) 0.4763(3) 0.0707(17) Uani 1 1 d . . . H14 H 0.0251 0.3154 0.4600 0.085 Uiso 1 1 calc R . . C15 C 0.2069(4) -0.0454(6) 0.5685(3) 0.0695(17) Uani 1 1 d . . . C16 C 0.2289(3) -0.1512(5) 0.5323(2) 0.0549(14) Uani 1 1 d . . . C17 C 0.1761(3) -0.2348(5) 0.5083(3) 0.0615(15) Uani 1 1 d . . . H17 H 0.1260 -0.2257 0.5142 0.074 Uiso 1 1 calc R . . C18 C 0.3033(3) -0.1676(5) 0.5246(3) 0.0657(16) Uani 1 1 d . . . H18 H 0.3399 -0.1122 0.5418 0.079 Uiso 1 1 calc R . . N1 N -0.0049(3) -0.0360(4) 0.6250(2) 0.0659(13) Uani 1 1 d . . . N2 N -0.1065(3) -0.1460(5) 0.5994(2) 0.0748(15) Uani 1 1 d . . . N3 N -0.2253(4) 0.1210(6) 0.7133(3) 0.0980(18) Uiso 1 1 d . . . N4 N -0.1375(3) 0.1097(5) 0.7964(2) 0.0774(15) Uani 1 1 d . . . O1 O 0.1373(2) -0.0348(4) 0.5704(2) 0.0877(14) Uani 1 1 d . . . O2 O 0.2554(3) 0.0259(4) 0.5947(2) 0.0953(15) Uani 1 1 d . . . O3 O 0.0549(2) 0.2028(4) 0.56028(19) 0.0766(12) Uani 1 1 d . . . O4 O 0.0011(3) 0.2918(4) 0.6340(3) 0.0971(15) Uani 1 1 d . . . O5 O -0.2491(3) -0.0520(6) 0.6148(3) 0.1261(19) Uiso 1 1 d . . . O1W' O -0.1264(6) -0.4436(9) 0.7033(5) 0.098(3) Uiso 0.50 1 d P . . O1W O -0.1200(6) -0.5368(11) 0.6684(5) 0.124(4) Uiso 0.50 1 d PD . . O2W O 0.0000 -0.5800(13) 0.7500 0.119(5) Uiso 0.50 2 d SPD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0577(5) 0.0647(5) 0.0692(5) -0.0093(4) 0.0068(3) 0.0069(4) C1 0.075(4) 0.068(4) 0.058(4) 0.006(3) 0.010(3) -0.006(4) C3 0.133(7) 0.083(5) 0.075(5) 0.028(4) 0.027(5) -0.010(5) C4 0.111(6) 0.099(6) 0.082(5) -0.028(4) 0.021(4) -0.038(5) C9 0.118(13) 0.070(11) 0.078(10) -0.016(8) 0.034(10) -0.027(10) C10 0.075(4) 0.099(5) 0.061(4) 0.015(4) 0.006(3) 0.005(4) C11 0.048(3) 0.069(5) 0.081(5) -0.008(4) 0.001(3) -0.005(3) C12 0.039(3) 0.065(4) 0.074(4) -0.010(3) 0.003(3) -0.002(3) C13 0.063(4) 0.067(4) 0.077(4) -0.008(4) 0.013(3) 0.006(3) C14 0.066(4) 0.052(4) 0.094(5) -0.010(4) 0.011(4) 0.007(3) C15 0.059(4) 0.081(5) 0.066(4) -0.009(3) 0.003(3) 0.007(4) C16 0.052(3) 0.056(4) 0.056(3) -0.004(3) 0.005(3) 0.006(3) C17 0.045(3) 0.067(4) 0.072(4) -0.007(3) 0.011(3) 0.002(3) C18 0.050(3) 0.059(4) 0.087(4) -0.013(3) 0.008(3) -0.004(3) N1 0.068(3) 0.067(3) 0.062(3) 0.006(3) 0.007(3) 0.002(3) N2 0.080(4) 0.083(4) 0.062(3) -0.011(3) 0.013(3) -0.023(3) N4 0.076(4) 0.088(4) 0.066(3) 0.015(3) 0.005(3) -0.015(3) O1 0.061(3) 0.093(3) 0.110(4) -0.033(3) 0.015(3) 0.016(3) O2 0.078(3) 0.084(3) 0.125(4) -0.044(3) 0.020(3) -0.001(3) O3 0.079(3) 0.067(3) 0.082(3) -0.002(2) 0.006(2) 0.018(2) O4 0.109(4) 0.082(3) 0.108(4) 0.006(3) 0.042(3) 0.010(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O3 1.921(4) . ? Zn1 O1 1.941(4) . ? Zn1 N4 1.977(5) 2_556 ? Zn1 N1 1.992(5) . ? C1 N2 1.306(7) . ? C1 N1 1.329(7) . ? C1 H1 0.9300 . ? C2 C3 1.331(9) . ? C2 N1 1.365(8) . ? C2 H2 0.9300 . ? C3 N2 1.354(8) . ? C3 H3 0.9300 . ? C4 N2 1.459(8) . ? C4 C5 1.489(9) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 O5 1.376(9) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 O5 1.414(9) . ? C6 C7 1.439(11) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 N3 1.509(9) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8' C8 0.76(2) . ? C8' N3 1.189(15) . ? C8' C9' 1.49(2) . ? C8 C9 1.39(2) . ? C8 C9' 1.45(2) . ? C8 N3 1.468(15) . ? C9 C9' 0.76(2) . ? C9 N4 1.472(15) . ? C9' N4 1.389(17) . ? C10 N4 1.307(7) . ? C10 N3 1.330(8) . ? C10 H10 0.9300 . ? C11 O4 1.212(7) . ? C11 O3 1.275(7) . ? C11 C12 1.516(8) . ? C12 C13 1.382(8) . ? C12 C14 1.384(8) . ? C13 C14 1.379(8) 5_566 ? C13 H13 0.9300 . ? C14 C13 1.379(8) 5_566 ? C14 H14 0.9300 . ? C15 O2 1.241(7) . ? C15 O1 1.258(7) . ? C15 C16 1.496(8) . ? C16 C17 1.364(7) . ? C16 C18 1.379(7) . ? C17 C18 1.377(7) 7_546 ? C17 H17 0.9300 . ? C18 C17 1.377(7) 7_546 ? C18 H18 0.9300 . ? N4 Zn1 1.977(5) 2_556 ? O1W' O1W 1.293(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Zn1 O1 102.7(2) . . ? O3 Zn1 N4 118.4(2) . 2_556 ? O1 Zn1 N4 113.4(2) . 2_556 ? O3 Zn1 N1 112.53(19) . . ? O1 Zn1 N1 97.9(2) . . ? N4 Zn1 N1 109.9(2) 2_556 . ? N2 C1 N1 112.1(6) . . ? N2 C1 H1 124.0 . . ? N1 C1 H1 124.0 . . ? C3 C2 N1 109.2(6) . . ? C3 C2 H2 125.4 . . ? N1 C2 H2 125.4 . . ? C2 C3 N2 107.4(6) . . ? C2 C3 H3 126.3 . . ? N2 C3 H3 126.3 . . ? N2 C4 C5 111.7(6) . . ? N2 C4 H4A 109.3 . . ? C5 C4 H4A 109.3 . . ? N2 C4 H4B 109.3 . . ? C5 C4 H4B 109.3 . . ? H4A C4 H4B 107.9 . . ? O5 C5 C4 108.8(7) . . ? O5 C5 H5A 109.9 . . ? C4 C5 H5A 109.9 . . ? O5 C5 H5B 109.9 . . ? C4 C5 H5B 109.9 . . ? H5A C5 H5B 108.3 . . ? O5 C6 C7 106.5(8) . . ? O5 C6 H6A 110.4 . . ? C7 C6 H6A 110.4 . . ? O5 C6 H6B 110.4 . . ? C7 C6 H6B 110.4 . . ? H6A C6 H6B 108.6 . . ? C6 C7 N3 111.9(7) . . ? C6 C7 H7A 109.2 . . ? N3 C7 H7A 109.2 . . ? C6 C7 H7B 109.2 . . ? N3 C7 H7B 109.2 . . ? H7A C7 H7B 107.9 . . ? C8 C8' N3 95(2) . . ? C8 C8' C9' 72(2) . . ? N3 C8' C9' 105.1(12) . . ? C8 C8' C9 47.6(18) . . ? N3 C8' C9 100.9(11) . . ? C8' C8 C9 109(2) . . ? C8' C8 C9' 78(2) . . ? C8' C8 N3 53.7(16) . . ? C9 C8 N3 108.6(11) . . ? C9' C8 N3 93.9(10) . . ? C9' C9 C8 79(3) . . ? C9' C9 N4 68.6(19) . . ? C8 C9 N4 102.7(12) . . ? C9' C9 C8' 56(2) . . ? N4 C9 C8' 89.1(11) . . ? C9 C9' N4 81(2) . . ? C9 C9' C8 70(2) . . ? N4 C9' C8 103.7(12) . . ? C9 C9' C8' 99(3) . . ? N4 C9' C8' 105.5(11) . . ? N4 C10 N3 111.4(6) . . ? N4 C10 H10 124.3 . . ? N3 C10 H10 124.3 . . ? O4 C11 O3 125.4(7) . . ? O4 C11 C12 120.2(6) . . ? O3 C11 C12 114.4(6) . . ? C13 C12 C14 118.3(6) . . ? C13 C12 C11 121.2(6) . . ? C14 C12 C11 120.5(6) . . ? C14 C13 C12 120.2(6) 5_566 . ? C14 C13 H13 119.9 5_566 . ? C12 C13 H13 119.9 . . ? C13 C14 C12 121.6(6) 5_566 . ? C13 C14 H14 119.2 5_566 . ? C12 C14 H14 119.2 . . ? O2 C15 O1 123.3(6) . . ? O2 C15 C16 121.0(6) . . ? O1 C15 C16 115.8(6) . . ? C17 C16 C18 119.2(5) . . ? C17 C16 C15 120.4(5) . . ? C18 C16 C15 120.3(5) . . ? C16 C17 C18 120.2(5) . 7_546 ? C16 C17 H17 119.9 . . ? C18 C17 H17 119.9 7_546 . ? C17 C18 C16 120.5(5) 7_546 . ? C17 C18 H18 119.7 7_546 . ? C16 C18 H18 119.7 . . ? C1 N1 C2 104.5(5) . . ? C1 N1 Zn1 129.6(4) . . ? C2 N1 Zn1 124.7(5) . . ? C1 N2 C3 106.8(5) . . ? C1 N2 C4 126.5(6) . . ? C3 N2 C4 126.7(6) . . ? C8' N3 C10 112.6(10) . . ? C10 N3 C8 105.4(8) . . ? C8' N3 C7 120.4(11) . . ? C10 N3 C7 126.1(7) . . ? C8 N3 C7 124.6(8) . . ? C10 N4 C9' 103.0(8) . . ? C10 N4 C9 109.5(8) . . ? C10 N4 Zn1 128.0(4) . 2_556 ? C9' N4 Zn1 127.4(8) . 2_556 ? C9 N4 Zn1 120.2(8) . 2_556 ? C15 O1 Zn1 131.6(4) . . ? C11 O3 Zn1 114.7(4) . . ? C5 O5 C6 112.8(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C2 C3 N2 -0.6(8) . . . . ? N2 C4 C5 O5 62.1(9) . . . . ? O5 C6 C7 N3 -66.2(9) . . . . ? N3 C8' C8 C9 -99.8(17) . . . . ? C9' C8' C8 C9 4.4(15) . . . . ? N3 C8' C8 C9' -104.2(13) . . . . ? C9 C8' C8 C9' -4.4(15) . . . . ? C9' C8' C8 N3 104.2(13) . . . . ? C9 C8' C8 N3 99.8(17) . . . . ? C8' C8 C9 C9' -8(3) . . . . ? N3 C8 C9 C9' -65(2) . . . . ? C8' C8 C9 N4 56(2) . . . . ? C9' C8 C9 N4 64.9(18) . . . . ? N3 C8 C9 N4 -0.5(17) . . . . ? C9' C8 C9 C8' 8(3) . . . . ? N3 C8 C9 C8' -56.9(17) . . . . ? C8 C8' C9 C9' 170(3) . . . . ? N3 C8' C9 C9' -103(2) . . . . ? N3 C8' C9 C8 87(2) . . . . ? C9' C8' C9 C8 -170(3) . . . . ? C8 C8' C9 N4 -126(2) . . . . ? N3 C8' C9 N4 -38.1(14) . . . . ? C9' C8' C9 N4 64(2) . . . . ? C8 C9 C9' N4 108.4(9) . . . . ? C8' C9 C9' N4 104.3(12) . . . . ? N4 C9 C9' C8 -108.4(9) . . . . ? C8' C9 C9' C8 -4.1(13) . . . . ? C8 C9 C9' C8' 4.1(13) . . . . ? N4 C9 C9' C8' -104.3(12) . . . . ? C8' C8 C9' C9 172(3) . . . . ? N3 C8 C9' C9 120(2) . . . . ? C8' C8 C9' N4 97(2) . . . . ? C9 C8 C9' N4 -75(2) . . . . ? N3 C8 C9' N4 45.8(15) . . . . ? C9 C8 C9' C8' -172(3) . . . . ? N3 C8 C9' C8' -51.6(15) . . . . ? C8 C8' C9' C9 -8(3) . . . . ? N3 C8' C9' C9 83(2) . . . . ? C8 C8' C9' N4 -91(2) . . . . ? N3 C8' C9' N4 0.4(19) . . . . ? C9 C8' C9' N4 -83(2) . . . . ? N3 C8' C9' C8 91(2) . . . . ? C9 C8' C9' C8 8(3) . . . . ? O4 C11 C12 C13 18.2(9) . . . . ? O3 C11 C12 C13 -161.1(5) . . . . ? O4 C11 C12 C14 -163.6(6) . . . . ? O3 C11 C12 C14 17.1(8) . . . . ? C14 C12 C13 C14 0.9(9) . . . 5_566 ? C11 C12 C13 C14 179.2(5) . . . 5_566 ? C13 C12 C14 C13 -0.9(9) . . . 5_566 ? C11 C12 C14 C13 -179.2(5) . . . 5_566 ? O2 C15 C16 C17 174.3(6) . . . . ? O1 C15 C16 C17 -5.6(9) . . . . ? O2 C15 C16 C18 -3.5(9) . . . . ? O1 C15 C16 C18 176.7(6) . . . . ? C18 C16 C17 C18 -1.7(10) . . . 7_546 ? C15 C16 C17 C18 -179.5(5) . . . 7_546 ? C17 C16 C18 C17 1.7(10) . . . 7_546 ? C15 C16 C18 C17 179.6(5) . . . 7_546 ? N2 C1 N1 C2 0.7(7) . . . . ? N2 C1 N1 Zn1 168.0(4) . . . . ? C3 C2 N1 C1 -0.1(8) . . . . ? C3 C2 N1 Zn1 -168.2(5) . . . . ? O3 Zn1 N1 C1 21.3(6) . . . . ? O1 Zn1 N1 C1 -86.0(5) . . . . ? N4 Zn1 N1 C1 155.5(5) 2_556 . . . ? O3 Zn1 N1 C2 -173.7(5) . . . . ? O1 Zn1 N1 C2 79.0(5) . . . . ? N4 Zn1 N1 C2 -39.4(6) 2_556 . . . ? N1 C1 N2 C3 -1.1(7) . . . . ? N1 C1 N2 C4 179.6(6) . . . . ? C2 C3 N2 C1 1.0(8) . . . . ? C2 C3 N2 C4 -179.7(6) . . . . ? C5 C4 N2 C1 -111.2(8) . . . . ? C5 C4 N2 C3 69.7(9) . . . . ? C8 C8' N3 C10 82(2) . . . . ? C9' C8' N3 C10 9.1(18) . . . . ? C9 C8' N3 C10 34.4(15) . . . . ? C9' C8' N3 C8 -73(2) . . . . ? C9 C8' N3 C8 -47.9(18) . . . . ? C8 C8' N3 C7 -108(2) . . . . ? C9' C8' N3 C7 179.3(10) . . . . ? C9 C8' N3 C7 -155.4(9) . . . . ? N4 C10 N3 C8' -16.5(14) . . . . ? N4 C10 N3 C8 15.3(11) . . . . ? N4 C10 N3 C7 173.9(7) . . . . ? C9 C8 N3 C8' 100(3) . . . . ? C9' C8 N3 C8' 72(2) . . . . ? C8' C8 N3 C10 -108(2) . . . . ? C9 C8 N3 C10 -8.6(16) . . . . ? C9' C8 N3 C10 -36.6(13) . . . . ? C8' C8 N3 C7 93(2) . . . . ? C9 C8 N3 C7 -167.6(11) . . . . ? C9' C8 N3 C7 164.3(10) . . . . ? C6 C7 N3 C8' 122.0(14) . . . . ? C6 C7 N3 C10 -69.2(10) . . . . ? C6 C7 N3 C8 85.5(13) . . . . ? N3 C10 N4 C9' 15.1(11) . . . . ? N3 C10 N4 C9 -16.2(11) . . . . ? N3 C10 N4 Zn1 -178.7(4) . . . 2_556 ? C9 C9' N4 C10 -106(2) . . . . ? C8 C9' N4 C10 -40.1(14) . . . . ? C8' C9' N4 C10 -9.3(15) . . . . ? C8 C9' N4 C9 66(2) . . . . ? C8' C9' N4 C9 97(2) . . . . ? C9 C9' N4 Zn1 87(2) . . . 2_556 ? C8 C9' N4 Zn1 153.7(10) . . . 2_556 ? C8' C9' N4 Zn1 -175.6(9) . . . 2_556 ? C9' C9 N4 C10 82(2) . . . . ? C8 C9 N4 C10 9.7(15) . . . . ? C8' C9 N4 C10 29.3(11) . . . . ? C8 C9 N4 C9' -73(3) . . . . ? C8' C9 N4 C9' -53(2) . . . . ? C9' C9 N4 Zn1 -113(2) . . . 2_556 ? C8 C9 N4 Zn1 173.8(10) . . . 2_556 ? C8' C9 N4 Zn1 -166.6(7) . . . 2_556 ? O2 C15 O1 Zn1 -8.3(11) . . . . ? C16 C15 O1 Zn1 171.6(4) . . . . ? O3 Zn1 O1 C15 94.2(6) . . . . ? N4 Zn1 O1 C15 -34.8(7) 2_556 . . . ? N1 Zn1 O1 C15 -150.5(6) . . . . ? O4 C11 O3 Zn1 -6.8(8) . . . . ? C12 C11 O3 Zn1 172.4(3) . . . . ? O1 Zn1 O3 C11 -175.6(4) . . . . ? N4 Zn1 O3 C11 -49.8(5) 2_556 . . . ? N1 Zn1 O3 C11 80.2(4) . . . . ? C4 C5 O5 C6 -179.2(7) . . . . ? C7 C6 O5 C5 169.1(7) . . . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.870 _refine_diff_density_min -0.448 _refine_diff_density_rms 0.084 #===END data_compound8 _database_code_depnum_ccdc_archive 'CCDC 665631' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H26 Cd3 N4 O13' _chemical_formula_sum 'C34 H26 Cd3 N4 O13' _chemical_formula_weight 1035.79 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 25.098(8) _cell_length_b 10.735(3) _cell_length_c 17.743(5) _cell_angle_alpha 90.00 _cell_angle_beta 128.707(9) _cell_angle_gamma 90.00 _cell_volume 3730(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3318 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.4 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.490 _exptl_crystal_size_mid 0.477 _exptl_crystal_size_min 0.055 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.844 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2024 _exptl_absorpt_coefficient_mu 1.764 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.434 _exptl_absorpt_correction_T_max 0.908 _exptl_absorpt_process_details ; Higashi,T (1995) Program for absorption correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17597 _diffrn_reflns_av_R_equivalents 0.0619 _diffrn_reflns_av_sigmaI/netI 0.0500 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 27.44 _reflns_number_total 4236 _reflns_number_gt 3322 _reflns_threshold_expression >2sigma(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction PROCESS-AUTO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0879P)^2^+19.6613P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00071(18) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4236 _refine_ls_number_parameters 245 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0740 _refine_ls_R_factor_gt 0.0573 _refine_ls_wR_factor_ref 0.1629 _refine_ls_wR_factor_gt 0.1468 _refine_ls_goodness_of_fit_ref 1.102 _refine_ls_restrained_S_all 1.102 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.32590(2) 0.67951(4) 0.61564(3) 0.02844(19) Uani 1 1 d . . . Cd2 Cd 0.5000 0.78078(6) 0.7500 0.0274(2) Uani 1 2 d S . . C1 C 0.3708(7) 0.4043(11) 0.6117(9) 0.130(7) Uani 1 1 d . . . H1 H 0.4061 0.4118 0.6776 0.157 Uiso 1 1 calc R . . C2 C 0.2835(5) 0.4412(10) 0.4699(7) 0.079(3) Uani 1 1 d . . . H2 H 0.2456 0.4812 0.4160 0.094 Uiso 1 1 calc R . . C3 C 0.3052(7) 0.3271(11) 0.4700(10) 0.118(6) Uani 1 1 d . . . H3 H 0.2849 0.2734 0.4176 0.142 Uiso 1 1 calc R . . C4' C 0.3913(11) 0.1727(19) 0.6135(15) 0.069(5) Uiso 0.50 1 d P . . C4 C 0.4198(12) 0.220(2) 0.5686(16) 0.078(6) Uiso 0.50 1 d P . . C5 C 0.4569(8) 0.1719(12) 0.6639(9) 0.108(5) Uani 1 1 d . . . C6 C 0.3918(3) 1.0842(6) 0.2608(4) 0.0340(14) Uani 1 1 d . . . C7 C 0.3804(3) 1.0110(7) 0.3225(4) 0.0368(15) Uani 1 1 d . . . C8 C 0.3189(4) 1.0183(8) 0.3060(5) 0.051(2) Uani 1 1 d . . . H8 H 0.2838 1.0668 0.2552 0.061 Uiso 1 1 calc R . . C9 C 0.3085(3) 0.9538(8) 0.3645(5) 0.050(2) Uani 1 1 d . . . H9 H 0.2668 0.9592 0.3524 0.061 Uiso 1 1 calc R . . C10 C 0.3611(3) 0.8815(7) 0.4410(4) 0.0343(14) Uani 1 1 d . . . C11 C 0.4227(4) 0.8746(8) 0.4577(5) 0.050(2) Uani 1 1 d . . . H11 H 0.4579 0.8265 0.5085 0.060 Uiso 1 1 calc R . . C12 C 0.4321(4) 0.9390(8) 0.3991(6) 0.055(2) Uani 1 1 d . . . H12 H 0.4739 0.9337 0.4113 0.065 Uiso 1 1 calc R . . C13 C 0.3515(3) 0.8135(6) 0.5041(4) 0.0292(13) Uani 1 1 d . . . C14 C 0.4184(3) 0.5928(7) 0.8041(4) 0.0374(15) Uani 1 1 d . . . C15 C 0.4614(3) 0.5446(7) 0.9062(4) 0.0373(15) Uani 1 1 d . . . C16 C 0.5310(4) 0.5384(9) 0.9617(5) 0.057(2) Uani 1 1 d . . . H16 H 0.5524 0.5650 0.9367 0.069 Uiso 1 1 calc R . . C17 C 0.4304(3) 0.5073(9) 0.9450(5) 0.056(2) Uani 1 1 d . . . H17 H 0.3832 0.5129 0.9080 0.067 Uiso 1 1 calc R . . N1 N 0.3250(3) 0.4894(7) 0.5599(5) 0.0576(18) Uani 1 1 d . . . N2 N 0.3617(6) 0.3057(10) 0.5605(8) 0.159(7) Uani 1 1 d . . . O1 O 0.3404(2) 1.1349(5) 0.1868(3) 0.0486(13) Uani 1 1 d . . . O2 O 0.4518(2) 1.0883(5) 0.2888(3) 0.0419(12) Uani 1 1 d . . . O3 O 0.4022(2) 0.7682(5) 0.5839(3) 0.0344(10) Uani 1 1 d . . . O4 O 0.2921(2) 0.7969(5) 0.4784(3) 0.0384(11) Uani 1 1 d . . . O5 O 0.4472(2) 0.6248(5) 0.7683(3) 0.0377(11) Uani 1 1 d . . . O6 O 0.3550(2) 0.5952(7) 0.7560(3) 0.0613(17) Uani 1 1 d . . . O7 O 0.5000 0.2412(10) 0.7500 0.099(4) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0208(3) 0.0373(3) 0.0192(2) 0.00505(15) 0.0086(2) 0.00201(16) Cd2 0.0198(3) 0.0364(4) 0.0234(3) 0.000 0.0122(3) 0.000 C1 0.097(9) 0.067(8) 0.081(8) -0.024(6) -0.016(6) 0.050(7) C2 0.063(6) 0.067(7) 0.052(5) -0.009(4) 0.009(5) 0.011(5) C3 0.081(8) 0.077(9) 0.099(9) -0.047(7) 0.008(7) 0.018(6) C5 0.122(12) 0.095(10) 0.079(8) 0.007(7) 0.050(8) 0.058(8) C6 0.035(3) 0.036(4) 0.031(3) 0.004(3) 0.021(3) 0.000(3) C7 0.028(3) 0.051(4) 0.030(3) 0.006(3) 0.017(3) -0.006(3) C8 0.029(3) 0.077(6) 0.040(4) 0.029(4) 0.019(3) 0.010(3) C9 0.025(3) 0.078(6) 0.049(4) 0.031(4) 0.024(3) 0.012(3) C10 0.021(3) 0.047(4) 0.027(3) 0.007(3) 0.011(3) 0.000(3) C11 0.032(4) 0.076(6) 0.049(4) 0.035(4) 0.028(3) 0.019(4) C12 0.032(4) 0.085(6) 0.056(4) 0.033(4) 0.033(4) 0.019(4) C13 0.029(3) 0.035(3) 0.023(3) -0.001(2) 0.016(3) -0.003(2) C14 0.031(3) 0.049(4) 0.024(3) 0.012(3) 0.013(3) 0.001(3) C15 0.029(3) 0.049(4) 0.028(3) 0.014(3) 0.015(3) -0.002(3) C16 0.030(4) 0.099(7) 0.035(4) 0.028(4) 0.016(3) 0.006(4) C17 0.022(3) 0.096(7) 0.037(4) 0.029(4) 0.012(3) -0.001(4) N1 0.049(4) 0.044(4) 0.045(4) -0.002(3) 0.013(3) 0.011(3) N2 0.091(7) 0.083(7) 0.113(9) -0.060(6) -0.028(6) 0.049(6) O1 0.040(3) 0.063(3) 0.033(2) 0.016(2) 0.019(2) -0.005(3) O2 0.036(2) 0.050(3) 0.051(3) 0.018(2) 0.033(2) 0.001(2) O3 0.023(2) 0.050(3) 0.024(2) 0.0069(19) 0.0119(18) 0.0032(19) O4 0.024(2) 0.056(3) 0.030(2) 0.015(2) 0.015(2) 0.002(2) O5 0.038(2) 0.043(3) 0.027(2) 0.0052(19) 0.018(2) -0.009(2) O6 0.029(3) 0.112(5) 0.030(2) 0.030(3) 0.012(2) 0.007(3) O7 0.059(6) 0.059(7) 0.124(10) 0.000 0.032(7) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N1 2.261(7) . ? Cd1 O1 2.262(5) 6_576 ? Cd1 O6 2.298(5) . ? Cd1 O4 2.332(4) 7_566 ? Cd1 O4 2.379(4) . ? Cd1 O3 2.497(4) . ? Cd1 O5 2.577(5) . ? Cd2 O2 2.226(4) 6_576 ? Cd2 O2 2.226(4) 5_676 ? Cd2 O5 2.281(4) . ? Cd2 O5 2.281(4) 2_656 ? Cd2 O3 2.383(4) . ? Cd2 O3 2.383(4) 2_656 ? C1 N1 1.296(11) . ? C1 N2 1.318(14) . ? C1 H1 0.9300 . ? C2 C3 1.340(14) . ? C2 N1 1.350(11) . ? C2 H2 0.9300 . ? C3 N2 1.340(15) . ? C3 H3 0.9300 . ? C4' C5 1.29(2) . ? C4' C4 1.46(3) . ? C4' N2 1.61(2) . ? C4 C5 1.42(2) . ? C4 N2 1.65(3) . ? C5 O7 1.410(14) . ? C6 O1 1.251(8) . ? C6 O2 1.259(8) . ? C6 C7 1.513(8) . ? C7 C8 1.382(9) . ? C7 C12 1.387(9) . ? C8 C9 1.401(9) . ? C8 H8 0.9300 . ? C9 C10 1.396(9) . ? C9 H9 0.9300 . ? C10 C11 1.380(9) . ? C10 C13 1.477(8) . ? C11 C12 1.388(9) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 O3 1.268(7) . ? C13 O4 1.270(7) . ? C14 O6 1.251(8) . ? C14 O5 1.272(8) . ? C14 C15 1.506(8) . ? C15 C16 1.369(10) . ? C15 C17 1.383(9) . ? C16 C17 1.384(9) 5_667 ? C16 H16 0.9300 . ? C17 C16 1.384(9) 5_667 ? C17 H17 0.9300 . ? O1 Cd1 2.262(5) 6_575 ? O2 Cd2 2.226(4) 5_676 ? O4 Cd1 2.332(4) 7_566 ? O7 C5 1.410(14) 2_656 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cd1 O1 173.0(2) . 6_576 ? N1 Cd1 O6 91.6(3) . . ? O1 Cd1 O6 84.9(2) 6_576 . ? N1 Cd1 O4 97.1(2) . 7_566 ? O1 Cd1 O4 89.62(18) 6_576 7_566 ? O6 Cd1 O4 102.60(16) . 7_566 ? N1 Cd1 O4 97.5(2) . . ? O1 Cd1 O4 86.24(18) 6_576 . ? O6 Cd1 O4 170.7(2) . . ? O4 Cd1 O4 74.34(17) 7_566 . ? N1 Cd1 O3 92.6(2) . . ? O1 Cd1 O3 84.89(18) 6_576 . ? O6 Cd1 O3 128.74(16) . . ? O4 Cd1 O3 127.39(14) 7_566 . ? O4 Cd1 O3 53.12(14) . . ? N1 Cd1 O5 86.3(2) . . ? O1 Cd1 O5 86.67(17) 6_576 . ? O6 Cd1 O5 53.51(15) . . ? O4 Cd1 O5 156.05(14) 7_566 . ? O4 Cd1 O5 128.88(14) . . ? O3 Cd1 O5 75.83(14) . . ? O2 Cd2 O2 101.7(3) 6_576 5_676 ? O2 Cd2 O5 86.76(18) 6_576 . ? O2 Cd2 O5 169.74(19) 5_676 . ? O2 Cd2 O5 169.74(19) 6_576 2_656 ? O2 Cd2 O5 86.76(18) 5_676 2_656 ? O5 Cd2 O5 85.5(3) . 2_656 ? O2 Cd2 O3 94.57(17) 6_576 . ? O2 Cd2 O3 89.53(17) 5_676 . ? O5 Cd2 O3 83.90(15) . . ? O5 Cd2 O3 91.33(16) 2_656 . ? O2 Cd2 O3 89.53(17) 6_576 2_656 ? O2 Cd2 O3 94.57(17) 5_676 2_656 ? O5 Cd2 O3 91.33(16) . 2_656 ? O5 Cd2 O3 83.90(15) 2_656 2_656 ? O3 Cd2 O3 173.5(2) . 2_656 ? N1 C1 N2 112.6(10) . . ? N1 C1 H1 123.7 . . ? N2 C1 H1 123.7 . . ? C3 C2 N1 109.7(9) . . ? C3 C2 H2 125.2 . . ? N1 C2 H2 125.2 . . ? N2 C3 C2 106.5(10) . . ? N2 C3 H3 126.7 . . ? C2 C3 H3 126.7 . . ? C5 C4' C4 62.1(15) . . ? C5 C4' N2 109.4(16) . . ? C4 C4' N2 64.8(14) . . ? C5 C4 C4' 53.2(13) . . ? C5 C4 N2 101.0(15) . . ? C4' C4 N2 62.2(13) . . ? C4' C5 O7 122.0(13) . . ? C4' C5 C4 64.7(14) . . ? O7 C5 C4 125.6(15) . . ? O1 C6 O2 126.3(6) . . ? O1 C6 C7 116.7(6) . . ? O2 C6 C7 117.0(5) . . ? C8 C7 C12 118.5(6) . . ? C8 C7 C6 120.6(6) . . ? C12 C7 C6 120.9(6) . . ? C7 C8 C9 121.0(6) . . ? C7 C8 H8 119.5 . . ? C9 C8 H8 119.5 . . ? C10 C9 C8 119.6(6) . . ? C10 C9 H9 120.2 . . ? C8 C9 H9 120.2 . . ? C11 C10 C9 119.4(6) . . ? C11 C10 C13 120.1(6) . . ? C9 C10 C13 120.5(6) . . ? C10 C11 C12 120.3(6) . . ? C10 C11 H11 119.8 . . ? C12 C11 H11 119.8 . . ? C7 C12 C11 121.1(6) . . ? C7 C12 H12 119.4 . . ? C11 C12 H12 119.4 . . ? O3 C13 O4 118.7(5) . . ? O3 C13 C10 120.7(5) . . ? O4 C13 C10 120.5(5) . . ? O6 C14 O5 122.2(5) . . ? O6 C14 C15 118.5(6) . . ? O5 C14 C15 119.3(6) . . ? C16 C15 C17 119.4(6) . . ? C16 C15 C14 121.0(6) . . ? C17 C15 C14 119.7(6) . . ? C15 C16 C17 120.1(7) . 5_667 ? C15 C16 H16 119.9 . . ? C17 C16 H16 119.9 5_667 . ? C15 C17 C16 120.5(7) . 5_667 ? C15 C17 H17 119.7 . . ? C16 C17 H17 119.7 5_667 . ? C1 N1 C2 104.7(8) . . ? C1 N1 Cd1 124.4(6) . . ? C2 N1 Cd1 130.7(6) . . ? C1 N2 C3 106.5(9) . . ? C1 N2 C4' 119.4(14) . . ? C3 N2 C4' 127.4(12) . . ? C1 N2 C4 128.5(13) . . ? C3 N2 C4 114.6(14) . . ? C4' N2 C4 53.0(11) . . ? C6 O1 Cd1 132.1(4) . 6_575 ? C6 O2 Cd2 130.4(4) . 5_676 ? C13 O3 Cd2 153.8(4) . . ? C13 O3 Cd1 91.3(3) . . ? Cd2 O3 Cd1 94.89(14) . . ? C13 O4 Cd1 157.3(4) . 7_566 ? C13 O4 Cd1 96.9(4) . . ? Cd1 O4 Cd1 105.66(17) 7_566 . ? C14 O5 Cd2 146.2(5) . . ? C14 O5 Cd1 85.4(4) . . ? Cd2 O5 Cd1 95.30(15) . . ? C14 O6 Cd1 98.8(4) . . ? C5 O7 C5 116.4(13) . 2_656 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C2 C3 N2 -2(2) . . . . ? N2 C4' C4 C5 131.7(15) . . . . ? C5 C4' C4 N2 -131.7(15) . . . . ? C4 C4' C5 O7 117.6(18) . . . . ? N2 C4' C5 O7 72(2) . . . . ? N2 C4' C5 C4 -45.8(15) . . . . ? N2 C4 C5 C4' 42.3(14) . . . . ? C4' C4 C5 O7 -112.5(18) . . . . ? N2 C4 C5 O7 -70(2) . . . . ? O1 C6 C7 C8 -10.5(11) . . . . ? O2 C6 C7 C8 169.5(7) . . . . ? O1 C6 C7 C12 171.9(7) . . . . ? O2 C6 C7 C12 -8.1(11) . . . . ? C12 C7 C8 C9 -0.5(13) . . . . ? C6 C7 C8 C9 -178.1(7) . . . . ? C7 C8 C9 C10 0.3(14) . . . . ? C8 C9 C10 C11 -0.1(13) . . . . ? C8 C9 C10 C13 179.5(7) . . . . ? C9 C10 C11 C12 0.1(13) . . . . ? C13 C10 C11 C12 -179.5(8) . . . . ? C8 C7 C12 C11 0.4(13) . . . . ? C6 C7 C12 C11 178.1(8) . . . . ? C10 C11 C12 C7 -0.2(14) . . . . ? C11 C10 C13 O3 13.5(10) . . . . ? C9 C10 C13 O3 -166.1(7) . . . . ? C11 C10 C13 O4 -164.9(7) . . . . ? C9 C10 C13 O4 15.5(10) . . . . ? O6 C14 C15 C16 179.2(8) . . . . ? O5 C14 C15 C16 2.1(12) . . . . ? O6 C14 C15 C17 -1.6(12) . . . . ? O5 C14 C15 C17 -178.7(8) . . . . ? C17 C15 C16 C17 1.4(16) . . . 5_667 ? C14 C15 C16 C17 -179.4(8) . . . 5_667 ? C16 C15 C17 C16 -1.4(16) . . . 5_667 ? C14 C15 C17 C16 179.4(8) . . . 5_667 ? N2 C1 N1 C2 1(2) . . . . ? N2 C1 N1 Cd1 -174.8(12) . . . . ? C3 C2 N1 C1 0.6(16) . . . . ? C3 C2 N1 Cd1 175.8(10) . . . . ? O6 Cd1 N1 C1 -43.2(12) . . . . ? O4 Cd1 N1 C1 -146.1(12) 7_566 . . . ? O4 Cd1 N1 C1 138.8(12) . . . . ? O3 Cd1 N1 C1 85.7(12) . . . . ? O5 Cd1 N1 C1 10.1(12) . . . . ? O6 Cd1 N1 C2 142.4(10) . . . . ? O4 Cd1 N1 C2 39.5(10) 7_566 . . . ? O4 Cd1 N1 C2 -35.6(10) . . . . ? O3 Cd1 N1 C2 -88.7(10) . . . . ? O5 Cd1 N1 C2 -164.3(10) . . . . ? N1 C1 N2 C3 -2(2) . . . . ? N1 C1 N2 C4' -155.2(16) . . . . ? N1 C1 N2 C4 140.5(17) . . . . ? C2 C3 N2 C1 2(2) . . . . ? C2 C3 N2 C4' 152.6(18) . . . . ? C2 C3 N2 C4 -146.3(15) . . . . ? C5 C4' N2 C1 -74(2) . . . . ? C4 C4' N2 C1 -118.1(19) . . . . ? C5 C4' N2 C3 139(2) . . . . ? C4 C4' N2 C3 95(2) . . . . ? C5 C4' N2 C4 44.4(15) . . . . ? C5 C4 N2 C1 63(2) . . . . ? C4' C4 N2 C1 101(2) . . . . ? C5 C4 N2 C3 -157.0(17) . . . . ? C4' C4 N2 C3 -119.5(17) . . . . ? C5 C4 N2 C4' -37.5(14) . . . . ? O2 C6 O1 Cd1 -38.0(11) . . . 6_575 ? C7 C6 O1 Cd1 141.9(5) . . . 6_575 ? O1 C6 O2 Cd2 18.7(11) . . . 5_676 ? C7 C6 O2 Cd2 -161.3(5) . . . 5_676 ? O4 C13 O3 Cd2 -103.7(9) . . . . ? C10 C13 O3 Cd2 77.8(11) . . . . ? O4 C13 O3 Cd1 0.2(6) . . . . ? C10 C13 O3 Cd1 -178.3(5) . . . . ? O2 Cd2 O3 C13 41.8(9) 6_576 . . . ? O2 Cd2 O3 C13 -59.8(9) 5_676 . . . ? O5 Cd2 O3 C13 128.1(9) . . . . ? O5 Cd2 O3 C13 -146.6(9) 2_656 . . . ? O2 Cd2 O3 Cd1 -61.30(18) 6_576 . . . ? O2 Cd2 O3 Cd1 -162.95(18) 5_676 . . . ? O5 Cd2 O3 Cd1 24.94(17) . . . . ? O5 Cd2 O3 Cd1 110.30(17) 2_656 . . . ? N1 Cd1 O3 C13 97.4(4) . . . . ? O1 Cd1 O3 C13 -89.2(4) 6_576 . . . ? O6 Cd1 O3 C13 -168.5(4) . . . . ? O4 Cd1 O3 C13 -3.6(4) 7_566 . . . ? O4 Cd1 O3 C13 -0.1(3) . . . . ? O5 Cd1 O3 C13 -177.1(4) . . . . ? N1 Cd1 O3 Cd2 -108.1(2) . . . . ? O1 Cd1 O3 Cd2 65.34(18) 6_576 . . . ? O6 Cd1 O3 Cd2 -13.9(3) . . . . ? O4 Cd1 O3 Cd2 150.94(17) 7_566 . . . ? O4 Cd1 O3 Cd2 154.5(3) . . . . ? O5 Cd1 O3 Cd2 -22.51(16) . . . . ? O3 C13 O4 Cd1 172.8(8) . . . 7_566 ? C10 C13 O4 Cd1 -8.8(15) . . . 7_566 ? O3 C13 O4 Cd1 -0.2(6) . . . . ? C10 C13 O4 Cd1 178.2(5) . . . . ? N1 Cd1 O4 C13 -87.5(4) . . . . ? O1 Cd1 O4 C13 86.5(4) 6_576 . . . ? O4 Cd1 O4 C13 177.2(5) 7_566 . . . ? O3 Cd1 O4 C13 0.1(4) . . . . ? O5 Cd1 O4 C13 3.9(5) . . . . ? N1 Cd1 O4 Cd1 95.3(2) . . . 7_566 ? O1 Cd1 O4 Cd1 -90.7(2) 6_576 . . 7_566 ? O4 Cd1 O4 Cd1 0.0 7_566 . . 7_566 ? O3 Cd1 O4 Cd1 -177.1(3) . . . 7_566 ? O5 Cd1 O4 Cd1 -173.32(16) . . . 7_566 ? O6 C14 O5 Cd2 96.1(9) . . . . ? C15 C14 O5 Cd2 -86.9(10) . . . . ? O6 C14 O5 Cd1 3.5(8) . . . . ? C15 C14 O5 Cd1 -179.5(6) . . . . ? O2 Cd2 O5 C14 -18.8(7) 6_576 . . . ? O2 Cd2 O5 C14 -164.2(9) 5_676 . . . ? O5 Cd2 O5 C14 154.4(8) 2_656 . . . ? O3 Cd2 O5 C14 -113.7(7) . . . . ? O3 Cd2 O5 C14 70.7(7) 2_656 . . . ? O2 Cd2 O5 Cd1 70.80(17) 6_576 . . . ? O2 Cd2 O5 Cd1 -74.6(10) 5_676 . . . ? O5 Cd2 O5 Cd1 -116.0(2) 2_656 . . . ? O3 Cd2 O5 Cd1 -24.14(16) . . . . ? O3 Cd2 O5 Cd1 160.26(16) 2_656 . . . ? N1 Cd1 O5 C14 -96.7(5) . . . . ? O1 Cd1 O5 C14 84.1(4) 6_576 . . . ? O6 Cd1 O5 C14 -2.0(4) . . . . ? O4 Cd1 O5 C14 2.6(7) 7_566 . . . ? O4 Cd1 O5 C14 166.6(4) . . . . ? O3 Cd1 O5 C14 169.7(4) . . . . ? N1 Cd1 O5 Cd2 117.2(2) . . . . ? O1 Cd1 O5 Cd2 -61.97(19) 6_576 . . . ? O6 Cd1 O5 Cd2 -148.1(3) . . . . ? O4 Cd1 O5 Cd2 -143.5(4) 7_566 . . . ? O4 Cd1 O5 Cd2 20.5(3) . . . . ? O3 Cd1 O5 Cd2 23.59(16) . . . . ? O5 C14 O6 Cd1 -4.0(9) . . . . ? C15 C14 O6 Cd1 179.1(6) . . . . ? N1 Cd1 O6 C14 86.3(5) . . . . ? O1 Cd1 O6 C14 -87.6(5) 6_576 . . . ? O3 Cd1 O6 C14 -8.3(7) . . . . ? O5 Cd1 O6 C14 2.1(5) . . . . ? C4' C5 O7 C5 113.3(19) . . . 2_656 ? C4 C5 O7 C5 -167(2) . . . 2_656 ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.369 _refine_diff_density_min -2.555 _refine_diff_density_rms 0.187 #===END data_compound9 _database_code_depnum_ccdc_archive 'CCDC 665632' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H35 Cd3 N8 O14.50' _chemical_formula_sum 'C38 H35 Cd3 N8 O14.50' _chemical_formula_weight 1172.94 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.474(6) _cell_length_b 13.589(3) _cell_length_c 19.478(5) _cell_angle_alpha 90.00 _cell_angle_beta 115.823(9) _cell_angle_gamma 90.00 _cell_volume 4163.5(19) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7117 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description Block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.490 _exptl_crystal_size_mid 0.477 _exptl_crystal_size_min 0.055 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.871 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2316 _exptl_absorpt_coefficient_mu 1.597 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.47 _exptl_absorpt_correction_T_max 0.9 _exptl_absorpt_process_details ; Higashi,T (1995) Program for absorption correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38555 _diffrn_reflns_av_R_equivalents 0.0685 _diffrn_reflns_av_sigmaI/netI 0.0588 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 27.48 _reflns_number_total 9431 _reflns_number_gt 7117 _reflns_threshold_expression >2sigma(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction PROCESS-AUTO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0348P)^2^+12.9169P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9431 _refine_ls_number_parameters 578 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0701 _refine_ls_R_factor_gt 0.0463 _refine_ls_wR_factor_ref 0.1011 _refine_ls_wR_factor_gt 0.0922 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.20631(2) 0.39970(3) 0.466410(18) 0.02055(9) Uani 1 1 d . . . Cd2 Cd 0.34792(2) 0.21264(3) 0.64417(2) 0.02658(10) Uani 1 1 d . . . Cd3 Cd 0.21441(2) 0.48906(3) 0.284204(19) 0.02329(9) Uani 1 1 d . . . C1 C 0.1124(3) 0.4156(4) 0.1071(3) 0.0310(12) Uani 1 1 d . . . H1 H 0.1625 0.4162 0.1013 0.037 Uiso 1 1 calc R . . C2 C 0.0232(4) 0.4320(5) 0.1538(3) 0.0495(17) Uani 1 1 d . . . H2 H -0.0002 0.4462 0.1874 0.059 Uiso 1 1 calc R . . C3 C -0.0206(4) 0.3946(6) 0.0826(4) 0.0548(19) Uani 1 1 d . . . H3 H -0.0783 0.3795 0.0585 0.066 Uiso 1 1 calc R . . C4 C 0.0208(4) 0.3470(5) -0.0223(3) 0.0430(15) Uani 1 1 d . . . H4A H 0.0735 0.3479 -0.0275 0.052 Uiso 1 1 calc R . . H4B H -0.0187 0.3911 -0.0604 0.052 Uiso 1 1 calc R . . C5 C -0.0151(4) 0.2446(5) -0.0378(4) 0.0506(17) Uani 1 1 d . . . H5A H -0.0170 0.2206 -0.0854 0.061 Uiso 1 1 calc R . . H5B H 0.0207 0.2007 0.0028 0.061 Uiso 1 1 calc R . . C6 C -0.1442(6) 0.1574(6) -0.0628(5) 0.088(3) Uani 1 1 d . . . H6A H -0.1896 0.1599 -0.0470 0.106 Uiso 1 1 calc R . . H6B H -0.1066 0.1038 -0.0355 0.106 Uiso 1 1 calc R . . C7 C -0.1799(7) 0.1370(7) -0.1426(5) 0.092(3) Uiso 1 1 d . . . H7A H -0.2162 0.0794 -0.1539 0.111 Uiso 1 1 calc R . . H7B H -0.1348 0.1232 -0.1576 0.111 Uiso 1 1 calc R . . C8 C -0.3160(7) 0.2485(7) -0.2109(5) 0.087(3) Uani 1 1 d . . . H8 H -0.3565 0.2118 -0.2032 0.105 Uiso 1 1 calc R . . C9 C -0.3284(5) 0.3355(6) -0.2473(4) 0.059(2) Uani 1 1 d . . . H9 H -0.3800 0.3686 -0.2710 0.070 Uiso 1 1 calc R . . C10 C -0.1967(5) 0.2984(5) -0.2088(4) 0.068(2) Uani 1 1 d . . . H10 H -0.1399 0.3008 -0.2000 0.082 Uiso 1 1 calc R . . C11 C 0.4174(5) 0.3617(5) 0.7952(4) 0.064(2) Uani 1 1 d . . . H11 H 0.4238 0.3122 0.8302 0.076 Uiso 1 1 calc R . . C12 C 0.3845(5) 0.4387(5) 0.6922(4) 0.0543(18) Uani 1 1 d . . . H12 H 0.3627 0.4533 0.6405 0.065 Uiso 1 1 calc R . . C13 C 0.4239(4) 0.5029(5) 0.7483(4) 0.0514(17) Uani 1 1 d . . . H13 H 0.4350 0.5686 0.7428 0.062 Uiso 1 1 calc R . . C14 C 0.4839(5) 0.4978(6) 0.8907(4) 0.069(2) Uani 1 1 d . . . H14A H 0.5389 0.5250 0.9000 0.083 Uiso 1 1 calc R . . H14B H 0.4929 0.4469 0.9283 0.083 Uiso 1 1 calc R . . C15 C 0.4294(6) 0.5771(6) 0.8991(4) 0.070(2) Uani 1 1 d . . . H15A H 0.4595 0.6108 0.9475 0.085 Uiso 1 1 calc R . . H15B H 0.4147 0.6248 0.8583 0.085 Uiso 1 1 calc R . . C16 C 0.2912(7) 0.6000(8) 0.8807(5) 0.092(3) Uani 1 1 d . . . H16A H 0.2720 0.6259 0.8295 0.110 Uiso 1 1 calc R . . H16B H 0.3113 0.6543 0.9166 0.110 Uiso 1 1 calc R . . C17 C 0.2187(5) 0.5458(7) 0.8887(4) 0.083(3) Uani 1 1 d . . . H17A H 0.1696 0.5886 0.8734 0.100 Uiso 1 1 calc R . . H17B H 0.2024 0.4883 0.8560 0.100 Uiso 1 1 calc R . . C18 C 0.2645(5) 0.5758(6) 1.0288(5) 0.066(2) Uani 1 1 d . . . H18 H 0.2556 0.6434 1.0273 0.079 Uiso 1 1 calc R . . C19 C 0.2970(5) 0.5184(5) 1.0913(4) 0.0561(18) Uani 1 1 d . . . H19 H 0.3152 0.5405 1.1411 0.067 Uiso 1 1 calc R . . C20 C 0.2679(4) 0.4244(5) 0.9955(3) 0.0418(15) Uani 1 1 d . . . H20 H 0.2610 0.3691 0.9653 0.050 Uiso 1 1 calc R . . C21 C 0.0642(3) 0.5420(4) 0.3402(3) 0.0262(11) Uani 1 1 d . . . C22 C -0.1750(3) 0.6594(4) 0.3961(3) 0.0244(11) Uani 1 1 d . . . C23 C -0.1522(3) 0.7753(4) 0.1589(3) 0.0232(10) Uani 1 1 d . . . C24 C -0.0188(3) 0.5969(4) 0.3153(2) 0.0221(10) Uani 1 1 d . . . C25 C -0.0631(3) 0.5949(4) 0.3599(3) 0.0242(10) Uani 1 1 d . . . H25 H -0.0446 0.5540 0.4024 0.029 Uiso 1 1 calc R . . C26 C -0.1343(3) 0.6528(4) 0.3417(3) 0.0221(10) Uani 1 1 d . . . C27 C -0.1632(3) 0.7136(4) 0.2770(3) 0.0233(10) Uani 1 1 d . . . H27 H -0.2098 0.7545 0.2658 0.028 Uiso 1 1 calc R . . C28 C -0.1219(3) 0.7127(4) 0.2293(3) 0.0236(10) Uani 1 1 d . . . C29 C -0.0495(3) 0.6544(4) 0.2495(3) 0.0250(11) Uani 1 1 d . . . H29 H -0.0213 0.6539 0.2185 0.030 Uiso 1 1 calc R . . C30 C 0.4094(3) 0.2932(4) 0.5468(3) 0.0268(11) Uani 1 1 d . . . C31 C 0.3921(3) 0.3845(4) 0.2910(3) 0.0241(10) Uani 1 1 d . . . C32 C 0.6612(3) 0.4487(4) 0.5297(3) 0.0252(11) Uani 1 1 d . . . C33 C 0.4503(3) 0.3348(4) 0.4996(3) 0.0236(10) Uani 1 1 d . . . C34 C 0.4032(3) 0.3460(4) 0.4211(3) 0.0232(10) Uani 1 1 d . . . H34 H 0.3459 0.3292 0.3981 0.028 Uiso 1 1 calc R . . C35 C 0.4417(3) 0.3821(4) 0.3770(3) 0.0227(10) Uani 1 1 d . . . C36 C 0.5270(3) 0.4109(4) 0.4117(3) 0.0234(10) Uani 1 1 d . . . H36 H 0.5530 0.4337 0.3821 0.028 Uiso 1 1 calc R . . C37 C 0.5729(3) 0.4055(4) 0.4906(3) 0.0220(10) Uani 1 1 d . . . C38 C 0.5351(3) 0.3651(4) 0.5334(3) 0.0253(11) Uani 1 1 d . . . H38 H 0.5668 0.3580 0.5858 0.030 Uiso 1 1 calc R . . N1 N 0.1062(3) 0.4460(3) 0.1690(2) 0.0291(10) Uani 1 1 d . . . N2 N 0.0373(3) 0.3837(4) 0.0538(2) 0.0361(11) Uani 1 1 d . . . N3 N -0.2313(6) 0.2241(5) -0.1871(4) 0.094(3) Uani 1 1 d . . . N4 N -0.2520(3) 0.3674(4) -0.2438(3) 0.0434(13) Uani 1 1 d . . . N5 N 0.3808(3) 0.3492(4) 0.7211(3) 0.0447(13) Uani 1 1 d . . . N6 N 0.4446(3) 0.4548(4) 0.8146(3) 0.0436(12) Uani 1 1 d . . . N7 N 0.2474(3) 0.5158(5) 0.9689(3) 0.0510(14) Uani 1 1 d . . . N8 N 0.2991(3) 0.4229(4) 1.0704(3) 0.0368(11) Uani 1 1 d . . . O1 O 0.1068(2) 0.5599(3) 0.3037(2) 0.0378(9) Uani 1 1 d . . . O2 O 0.0855(2) 0.4866(3) 0.3969(2) 0.0407(10) Uani 1 1 d . . . O3 O -0.1668(2) 0.5861(3) 0.43846(19) 0.0304(8) Uani 1 1 d . . . O4 O -0.2114(2) 0.7378(3) 0.3979(2) 0.0329(9) Uani 1 1 d . . . O5 O -0.2002(2) 0.8487(3) 0.15302(18) 0.0242(7) Uani 1 1 d . . . O6 O -0.1304(2) 0.7556(3) 0.1074(2) 0.0335(9) Uani 1 1 d . . . O7 O 0.3294(2) 0.2956(3) 0.5219(2) 0.0305(8) Uani 1 1 d . . . O8 O 0.4566(2) 0.2552(3) 0.6101(2) 0.0402(10) Uani 1 1 d . . . O9 O 0.3128(2) 0.3975(3) 0.26076(18) 0.0319(8) Uani 1 1 d . . . O10 O 0.4333(2) 0.3683(3) 0.25304(19) 0.0356(9) Uani 1 1 d . . . O11 O 0.6935(2) 0.4513(3) 0.6005(2) 0.0416(10) Uani 1 1 d . . . O12 O 0.6941(2) 0.4820(3) 0.4888(2) 0.0356(9) Uani 1 1 d . . . O13 O -0.0981(3) 0.2468(3) -0.0422(2) 0.0516(12) Uani 1 1 d . . . O14 O 0.3556(4) 0.5319(4) 0.8961(4) 0.0784(17) Uani 1 1 d . . . O1W O 0.1830(10) 0.7703(10) 0.9070(9) 0.107(5) Uani 0.50 1 d PD . . H1A H 0.210(11) 0.772(19) 0.879(10) 0.161 Uiso 0.50 1 d PD . . H1B H 0.131(4) 0.758(19) 0.878(10) 0.161 Uiso 0.50 1 d PD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.01600(16) 0.03046(19) 0.01632(16) -0.00058(15) 0.00808(12) 0.00030(14) Cd2 0.02523(19) 0.0360(2) 0.02017(17) 0.00318(16) 0.01140(14) 0.00316(15) Cd3 0.01843(17) 0.0336(2) 0.01841(17) 0.00138(16) 0.00856(13) 0.00016(14) C1 0.025(3) 0.037(3) 0.030(3) -0.001(2) 0.011(2) 0.004(2) C2 0.034(3) 0.080(5) 0.039(3) -0.019(3) 0.020(3) -0.011(3) C3 0.026(3) 0.093(6) 0.046(4) -0.028(4) 0.016(3) -0.011(3) C4 0.039(3) 0.061(4) 0.024(3) -0.004(3) 0.009(2) 0.007(3) C5 0.052(4) 0.046(4) 0.038(3) -0.006(3) 0.005(3) 0.008(3) C6 0.117(8) 0.053(5) 0.064(5) 0.006(4) 0.010(5) -0.026(5) C8 0.115(8) 0.085(6) 0.055(5) -0.012(5) 0.029(5) -0.070(6) C9 0.071(5) 0.067(5) 0.040(4) -0.005(4) 0.026(4) -0.025(4) C10 0.070(5) 0.051(4) 0.045(4) 0.013(4) -0.010(4) -0.021(4) C11 0.100(6) 0.050(4) 0.031(3) 0.008(3) 0.020(4) -0.018(4) C12 0.073(5) 0.050(4) 0.040(4) 0.000(3) 0.024(3) -0.015(4) C13 0.065(5) 0.047(4) 0.047(4) -0.003(3) 0.029(3) -0.022(3) C14 0.072(5) 0.082(6) 0.042(4) -0.016(4) 0.015(4) -0.022(5) C15 0.102(7) 0.070(5) 0.052(4) -0.015(4) 0.045(5) -0.020(5) C16 0.117(8) 0.096(7) 0.082(6) 0.043(6) 0.060(6) 0.002(6) C17 0.074(6) 0.111(7) 0.051(5) 0.042(5) 0.016(4) 0.009(5) C18 0.078(6) 0.047(4) 0.084(6) 0.020(4) 0.046(5) 0.022(4) C19 0.081(5) 0.046(4) 0.050(4) -0.005(3) 0.037(4) 0.009(4) C20 0.046(4) 0.042(4) 0.031(3) 0.005(3) 0.011(3) -0.004(3) C21 0.019(2) 0.034(3) 0.026(2) -0.002(2) 0.010(2) 0.007(2) C22 0.019(2) 0.038(3) 0.020(2) 0.000(2) 0.0117(19) 0.000(2) C23 0.018(2) 0.034(3) 0.016(2) 0.004(2) 0.0063(18) 0.001(2) C24 0.019(2) 0.032(3) 0.014(2) 0.002(2) 0.0061(18) 0.006(2) C25 0.028(3) 0.028(3) 0.021(2) 0.003(2) 0.015(2) 0.003(2) C26 0.020(2) 0.029(3) 0.020(2) 0.001(2) 0.0112(19) 0.0022(19) C27 0.019(2) 0.027(3) 0.022(2) 0.003(2) 0.0078(19) 0.0063(19) C28 0.022(2) 0.030(3) 0.018(2) -0.003(2) 0.0086(19) 0.001(2) C29 0.025(3) 0.037(3) 0.020(2) 0.007(2) 0.016(2) 0.006(2) C30 0.025(3) 0.033(3) 0.025(2) -0.002(2) 0.013(2) 0.000(2) C31 0.020(2) 0.033(3) 0.021(2) -0.004(2) 0.0093(19) -0.008(2) C32 0.020(2) 0.030(3) 0.023(2) -0.002(2) 0.007(2) -0.002(2) C33 0.021(2) 0.030(3) 0.022(2) -0.001(2) 0.0120(19) 0.002(2) C34 0.015(2) 0.031(3) 0.023(2) -0.001(2) 0.0084(18) -0.0026(19) C35 0.018(2) 0.031(3) 0.018(2) -0.005(2) 0.0075(18) 0.0006(19) C36 0.023(2) 0.032(3) 0.018(2) -0.003(2) 0.0120(19) -0.004(2) C37 0.017(2) 0.030(3) 0.019(2) -0.003(2) 0.0077(18) -0.0014(19) C38 0.025(3) 0.029(3) 0.021(2) -0.004(2) 0.009(2) -0.001(2) N1 0.023(2) 0.037(2) 0.026(2) -0.002(2) 0.0094(18) 0.0004(18) N2 0.028(2) 0.050(3) 0.027(2) -0.010(2) 0.0092(19) -0.002(2) N3 0.121(7) 0.057(4) 0.044(4) 0.018(3) -0.021(4) -0.046(4) N4 0.052(3) 0.044(3) 0.024(2) 0.006(2) 0.008(2) -0.013(2) N5 0.061(4) 0.041(3) 0.033(3) 0.003(2) 0.021(2) -0.011(3) N6 0.050(3) 0.046(3) 0.035(3) -0.005(2) 0.018(2) -0.009(2) N7 0.039(3) 0.071(4) 0.045(3) 0.021(3) 0.019(2) 0.004(3) N8 0.037(3) 0.044(3) 0.031(2) -0.004(2) 0.018(2) -0.002(2) O1 0.030(2) 0.055(3) 0.036(2) 0.0090(19) 0.0209(17) 0.0149(18) O2 0.031(2) 0.060(3) 0.036(2) 0.021(2) 0.0186(17) 0.0234(19) O3 0.039(2) 0.037(2) 0.0257(18) 0.0054(17) 0.0238(16) 0.0025(16) O4 0.029(2) 0.038(2) 0.041(2) 0.0007(18) 0.0232(17) 0.0069(16) O5 0.0182(16) 0.0331(19) 0.0212(16) 0.0025(15) 0.0086(13) 0.0073(14) O6 0.038(2) 0.043(2) 0.0259(18) 0.0052(17) 0.0201(17) 0.0118(17) O7 0.0207(17) 0.041(2) 0.0327(19) 0.0070(17) 0.0146(15) 0.0023(15) O8 0.030(2) 0.063(3) 0.028(2) 0.019(2) 0.0130(17) 0.0047(19) O9 0.0187(17) 0.056(2) 0.0179(16) 0.0004(17) 0.0047(14) -0.0008(16) O10 0.0259(19) 0.062(3) 0.0238(18) -0.0099(18) 0.0151(15) -0.0076(18) O11 0.029(2) 0.064(3) 0.0213(18) -0.0028(19) 0.0016(16) -0.0150(19) O12 0.028(2) 0.046(2) 0.032(2) 0.0002(18) 0.0123(16) -0.0125(17) O13 0.055(3) 0.049(3) 0.042(2) -0.004(2) 0.012(2) -0.007(2) O14 0.111(5) 0.068(4) 0.092(4) 0.002(3) 0.078(4) -0.010(4) O1W 0.109(11) 0.056(7) 0.158(13) 0.061(9) 0.059(10) 0.040(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O12 2.247(4) 3_666 ? Cd1 O3 2.250(3) 3_566 ? Cd1 O2 2.278(4) . ? Cd1 O5 2.385(3) 2_545 ? Cd1 O7 2.403(3) . ? Cd1 O6 2.450(4) 2_545 ? Cd2 O4 2.261(4) 3_566 ? Cd2 N8 2.262(5) 4_565 ? Cd2 O10 2.275(4) 4_566 ? Cd2 N5 2.295(5) . ? Cd2 O8 2.341(4) . ? Cd2 O7 2.525(4) . ? Cd3 O11 2.267(3) 3_666 ? Cd3 O1 2.285(4) . ? Cd3 N1 2.293(4) . ? Cd3 N4 2.304(5) 3_565 ? Cd3 O9 2.322(4) . ? Cd3 O5 2.337(3) 2_545 ? C1 N1 1.322(7) . ? C1 N2 1.342(7) . ? C1 H1 0.9300 . ? C2 C3 1.357(8) . ? C2 N1 1.362(7) . ? C2 H2 0.9300 . ? C3 N2 1.362(8) . ? C3 H3 0.9300 . ? C4 N2 1.468(7) . ? C4 C5 1.502(9) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 O13 1.415(8) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 O13 1.415(8) . ? C6 C7 1.427(11) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 N3 1.510(11) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.348(11) . ? C8 N3 1.385(13) . ? C8 H8 0.9300 . ? C9 N4 1.376(9) . ? C9 H9 0.9300 . ? C10 N4 1.305(9) . ? C10 N3 1.337(10) . ? C10 H10 0.9300 . ? C11 N5 1.311(8) . ? C11 N6 1.346(8) . ? C11 H11 0.9300 . ? C12 C13 1.331(9) . ? C12 N5 1.354(8) . ? C12 H12 0.9300 . ? C13 N6 1.349(8) . ? C13 H13 0.9300 . ? C14 N6 1.458(8) . ? C14 C15 1.492(11) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 O14 1.406(9) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 O14 1.386(11) . ? C16 C17 1.531(12) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 N7 1.474(8) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C19 1.344(10) . ? C18 N7 1.346(9) . ? C18 H18 0.9300 . ? C19 N8 1.365(8) . ? C19 H19 0.9300 . ? C20 N8 1.316(7) . ? C20 N7 1.333(8) . ? C20 H20 0.9300 . ? C21 O2 1.253(6) . ? C21 O1 1.258(6) . ? C21 C24 1.511(6) . ? C22 O4 1.249(6) . ? C22 O3 1.261(6) . ? C22 C26 1.514(6) . ? C23 O6 1.247(6) . ? C23 O5 1.276(6) . ? C23 C28 1.501(7) . ? C24 C25 1.392(6) . ? C24 C29 1.393(6) . ? C25 C26 1.381(7) . ? C25 H25 0.9300 . ? C26 C27 1.403(7) . ? C27 C28 1.402(7) . ? C27 H27 0.9300 . ? C28 C29 1.397(7) . ? C29 H29 0.9300 . ? C30 O8 1.257(6) . ? C30 O7 1.265(6) . ? C30 C33 1.499(7) . ? C31 O10 1.255(6) . ? C31 O9 1.261(6) . ? C31 C35 1.515(6) . ? C32 O11 1.242(6) . ? C32 O12 1.253(6) . ? C32 C37 1.511(6) . ? C33 C34 1.394(6) . ? C33 C38 1.397(7) . ? C34 C35 1.391(7) . ? C34 H34 0.9300 . ? C35 C36 1.396(6) . ? C36 C37 1.393(6) . ? C36 H36 0.9300 . ? C37 C38 1.382(7) . ? C38 H38 0.9300 . ? N4 Cd3 2.304(5) 3_565 ? N8 Cd2 2.262(5) 4_566 ? O3 Cd1 2.250(3) 3_566 ? O4 Cd2 2.261(4) 3_566 ? O5 Cd3 2.337(3) 2 ? O5 Cd1 2.385(3) 2 ? O6 Cd1 2.450(4) 2 ? O10 Cd2 2.275(4) 4_565 ? O11 Cd3 2.267(3) 3_666 ? O12 Cd1 2.247(4) 3_666 ? O1W H1A 0.86(3) . ? O1W H1B 0.86(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O12 Cd1 O3 94.73(14) 3_666 3_566 ? O12 Cd1 O2 102.73(15) 3_666 . ? O3 Cd1 O2 84.71(13) 3_566 . ? O12 Cd1 O5 106.55(12) 3_666 2_545 ? O3 Cd1 O5 158.25(12) 3_566 2_545 ? O2 Cd1 O5 86.25(13) . 2_545 ? O12 Cd1 O7 81.73(14) 3_666 . ? O3 Cd1 O7 102.46(13) 3_566 . ? O2 Cd1 O7 171.34(14) . . ? O5 Cd1 O7 85.35(12) 2_545 . ? O12 Cd1 O6 158.33(13) 3_666 2_545 ? O3 Cd1 O6 105.67(13) 3_566 2_545 ? O2 Cd1 O6 86.63(15) . 2_545 ? O5 Cd1 O6 54.00(11) 2_545 2_545 ? O7 Cd1 O6 86.72(13) . 2_545 ? O4 Cd2 N8 88.06(15) 3_566 4_565 ? O4 Cd2 O10 129.93(13) 3_566 4_566 ? N8 Cd2 O10 96.37(16) 4_565 4_566 ? O4 Cd2 N5 85.43(17) 3_566 . ? N8 Cd2 N5 172.24(18) 4_565 . ? O10 Cd2 N5 84.63(16) 4_566 . ? O4 Cd2 O8 132.95(13) 3_566 . ? N8 Cd2 O8 98.58(16) 4_565 . ? O10 Cd2 O8 95.76(13) 4_566 . ? N5 Cd2 O8 88.96(17) . . ? O4 Cd2 O7 81.01(12) 3_566 . ? N8 Cd2 O7 84.65(15) 4_565 . ? O10 Cd2 O7 149.03(12) 4_566 . ? N5 Cd2 O7 98.47(15) . . ? O8 Cd2 O7 53.73(11) . . ? O11 Cd3 O1 88.03(15) 3_666 . ? O11 Cd3 N1 170.96(16) 3_666 . ? O1 Cd3 N1 83.27(15) . . ? O11 Cd3 N4 81.41(16) 3_666 3_565 ? O1 Cd3 N4 94.45(18) . 3_565 ? N1 Cd3 N4 96.78(16) . 3_565 ? O11 Cd3 O9 96.85(14) 3_666 . ? O1 Cd3 O9 172.17(14) . . ? N1 Cd3 O9 92.06(14) . . ? N4 Cd3 O9 92.34(17) 3_565 . ? O11 Cd3 O5 87.98(13) 3_666 2_545 ? O1 Cd3 O5 88.52(13) . 2_545 ? N1 Cd3 O5 94.23(14) . 2_545 ? N4 Cd3 O5 168.86(14) 3_565 2_545 ? O9 Cd3 O5 85.55(13) . 2_545 ? N1 C1 N2 111.5(5) . . ? N1 C1 H1 124.3 . . ? N2 C1 H1 124.3 . . ? C3 C2 N1 110.4(5) . . ? C3 C2 H2 124.8 . . ? N1 C2 H2 124.8 . . ? C2 C3 N2 105.8(5) . . ? C2 C3 H3 127.1 . . ? N2 C3 H3 127.1 . . ? N2 C4 C5 113.5(5) . . ? N2 C4 H4A 108.9 . . ? C5 C4 H4A 108.9 . . ? N2 C4 H4B 108.9 . . ? C5 C4 H4B 108.9 . . ? H4A C4 H4B 107.7 . . ? O13 C5 C4 108.6(5) . . ? O13 C5 H5A 110.0 . . ? C4 C5 H5A 110.0 . . ? O13 C5 H5B 110.0 . . ? C4 C5 H5B 110.0 . . ? H5A C5 H5B 108.3 . . ? O13 C6 C7 113.7(8) . . ? O13 C6 H6A 108.8 . . ? C7 C6 H6A 108.8 . . ? O13 C6 H6B 108.8 . . ? C7 C6 H6B 108.8 . . ? H6A C6 H6B 107.7 . . ? C6 C7 N3 109.9(8) . . ? C6 C7 H7A 109.7 . . ? N3 C7 H7A 109.7 . . ? C6 C7 H7B 109.7 . . ? N3 C7 H7B 109.7 . . ? H7A C7 H7B 108.2 . . ? C9 C8 N3 106.8(7) . . ? C9 C8 H8 126.6 . . ? N3 C8 H8 126.6 . . ? C8 C9 N4 108.6(8) . . ? C8 C9 H9 125.7 . . ? N4 C9 H9 125.7 . . ? N4 C10 N3 111.9(8) . . ? N4 C10 H10 124.1 . . ? N3 C10 H10 124.1 . . ? N5 C11 N6 112.0(6) . . ? N5 C11 H11 124.0 . . ? N6 C11 H11 124.0 . . ? C13 C12 N5 110.5(6) . . ? C13 C12 H12 124.8 . . ? N5 C12 H12 124.8 . . ? C12 C13 N6 107.1(6) . . ? C12 C13 H13 126.4 . . ? N6 C13 H13 126.4 . . ? N6 C14 C15 111.2(6) . . ? N6 C14 H14A 109.4 . . ? C15 C14 H14A 109.4 . . ? N6 C14 H14B 109.4 . . ? C15 C14 H14B 109.4 . . ? H14A C14 H14B 108.0 . . ? O14 C15 C14 107.3(7) . . ? O14 C15 H15A 110.3 . . ? C14 C15 H15A 110.3 . . ? O14 C15 H15B 110.3 . . ? C14 C15 H15B 110.3 . . ? H15A C15 H15B 108.5 . . ? O14 C16 C17 106.6(7) . . ? O14 C16 H16A 110.4 . . ? C17 C16 H16A 110.4 . . ? O14 C16 H16B 110.4 . . ? C17 C16 H16B 110.4 . . ? H16A C16 H16B 108.6 . . ? N7 C17 C16 109.0(7) . . ? N7 C17 H17A 109.9 . . ? C16 C17 H17A 109.9 . . ? N7 C17 H17B 109.9 . . ? C16 C17 H17B 109.9 . . ? H17A C17 H17B 108.3 . . ? C19 C18 N7 106.3(6) . . ? C19 C18 H18 126.8 . . ? N7 C18 H18 126.8 . . ? C18 C19 N8 109.7(6) . . ? C18 C19 H19 125.2 . . ? N8 C19 H19 125.2 . . ? N8 C20 N7 110.9(6) . . ? N8 C20 H20 124.5 . . ? N7 C20 H20 124.5 . . ? O2 C21 O1 126.4(5) . . ? O2 C21 C24 117.1(4) . . ? O1 C21 C24 116.5(4) . . ? O4 C22 O3 124.6(4) . . ? O4 C22 C26 118.1(4) . . ? O3 C22 C26 117.2(4) . . ? O6 C23 O5 121.0(4) . . ? O6 C23 C28 120.3(4) . . ? O5 C23 C28 118.8(4) . . ? C25 C24 C29 119.3(4) . . ? C25 C24 C21 120.5(4) . . ? C29 C24 C21 120.1(4) . . ? C26 C25 C24 120.8(4) . . ? C26 C25 H25 119.6 . . ? C24 C25 H25 119.6 . . ? C25 C26 C27 119.8(4) . . ? C25 C26 C22 119.9(4) . . ? C27 C26 C22 119.9(4) . . ? C28 C27 C26 120.1(4) . . ? C28 C27 H27 119.9 . . ? C26 C27 H27 119.9 . . ? C29 C28 C27 118.9(4) . . ? C29 C28 C23 119.6(4) . . ? C27 C28 C23 121.5(4) . . ? C24 C29 C28 121.0(4) . . ? C24 C29 H29 119.5 . . ? C28 C29 H29 119.5 . . ? O8 C30 O7 122.0(5) . . ? O8 C30 C33 118.2(4) . . ? O7 C30 C33 119.8(4) . . ? O10 C31 O9 123.1(4) . . ? O10 C31 C35 116.7(4) . . ? O9 C31 C35 120.2(4) . . ? O11 C32 O12 125.7(5) . . ? O11 C32 C37 116.2(4) . . ? O12 C32 C37 118.1(4) . . ? C34 C33 C38 118.9(4) . . ? C34 C33 C30 120.2(4) . . ? C38 C33 C30 120.9(4) . . ? C35 C34 C33 120.2(4) . . ? C35 C34 H34 119.9 . . ? C33 C34 H34 119.9 . . ? C34 C35 C36 120.1(4) . . ? C34 C35 C31 119.5(4) . . ? C36 C35 C31 120.3(4) . . ? C37 C36 C35 120.0(4) . . ? C37 C36 H36 120.0 . . ? C35 C36 H36 120.0 . . ? C38 C37 C36 119.3(4) . . ? C38 C37 C32 120.1(4) . . ? C36 C37 C32 120.4(4) . . ? C37 C38 C33 121.3(4) . . ? C37 C38 H38 119.3 . . ? C33 C38 H38 119.3 . . ? C1 N1 C2 105.1(4) . . ? C1 N1 Cd3 127.8(3) . . ? C2 N1 Cd3 126.5(4) . . ? C1 N2 C3 107.3(5) . . ? C1 N2 C4 125.9(5) . . ? C3 N2 C4 126.7(5) . . ? C10 N3 C8 106.2(7) . . ? C10 N3 C7 122.4(9) . . ? C8 N3 C7 131.4(8) . . ? C10 N4 C9 106.4(6) . . ? C10 N4 Cd3 122.0(5) . 3_565 ? C9 N4 Cd3 131.6(5) . 3_565 ? C11 N5 C12 104.6(6) . . ? C11 N5 Cd2 133.4(5) . . ? C12 N5 Cd2 120.0(4) . . ? C11 N6 C13 105.8(5) . . ? C11 N6 C14 128.0(6) . . ? C13 N6 C14 126.2(6) . . ? C20 N7 C18 107.8(5) . . ? C20 N7 C17 125.4(7) . . ? C18 N7 C17 126.5(7) . . ? C20 N8 C19 105.3(5) . . ? C20 N8 Cd2 125.1(4) . 4_566 ? C19 N8 Cd2 129.6(4) . 4_566 ? C21 O1 Cd3 138.2(4) . . ? C21 O2 Cd1 132.7(3) . . ? C22 O3 Cd1 118.9(3) . 3_566 ? C22 O4 Cd2 135.5(3) . 3_566 ? C23 O5 Cd3 143.8(3) . 2 ? C23 O5 Cd1 93.6(3) . 2 ? Cd3 O5 Cd1 107.67(13) 2 2 ? C23 O6 Cd1 91.4(3) . 2 ? C30 O7 Cd1 144.2(3) . . ? C30 O7 Cd2 87.8(3) . . ? Cd1 O7 Cd2 114.13(13) . . ? C30 O8 Cd2 96.5(3) . . ? C31 O9 Cd3 137.8(3) . . ? C31 O10 Cd2 108.8(3) . 4_565 ? C32 O11 Cd3 153.2(4) . 3_666 ? C32 O12 Cd1 120.2(3) . 3_666 ? C6 O13 C5 116.1(6) . . ? C16 O14 C15 111.2(7) . . ? H1A O1W H1B 107(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C2 C3 N2 1.0(9) . . . . ? N2 C4 C5 O13 67.8(6) . . . . ? O13 C6 C7 N3 -52.5(12) . . . . ? N3 C8 C9 N4 -2.4(9) . . . . ? N5 C12 C13 N6 -1.2(9) . . . . ? N6 C14 C15 O14 67.3(8) . . . . ? O14 C16 C17 N7 65.5(10) . . . . ? N7 C18 C19 N8 -0.8(9) . . . . ? O2 C21 C24 C25 7.9(7) . . . . ? O1 C21 C24 C25 -169.1(5) . . . . ? O2 C21 C24 C29 -175.4(5) . . . . ? O1 C21 C24 C29 7.6(7) . . . . ? C29 C24 C25 C26 -3.3(8) . . . . ? C21 C24 C25 C26 173.4(5) . . . . ? C24 C25 C26 C27 0.8(8) . . . . ? C24 C25 C26 C22 -172.2(5) . . . . ? O4 C22 C26 C25 149.1(5) . . . . ? O3 C22 C26 C25 -28.3(7) . . . . ? O4 C22 C26 C27 -23.9(7) . . . . ? O3 C22 C26 C27 158.7(5) . . . . ? C25 C26 C27 C28 2.5(7) . . . . ? C22 C26 C27 C28 175.6(4) . . . . ? C26 C27 C28 C29 -3.3(7) . . . . ? C26 C27 C28 C23 178.8(4) . . . . ? O6 C23 C28 C29 21.0(7) . . . . ? O5 C23 C28 C29 -158.8(5) . . . . ? O6 C23 C28 C27 -161.0(5) . . . . ? O5 C23 C28 C27 19.2(7) . . . . ? C25 C24 C29 C28 2.5(8) . . . . ? C21 C24 C29 C28 -174.2(5) . . . . ? C27 C28 C29 C24 0.7(8) . . . . ? C23 C28 C29 C24 178.7(5) . . . . ? O8 C30 C33 C34 157.7(5) . . . . ? O7 C30 C33 C34 -21.2(7) . . . . ? O8 C30 C33 C38 -23.9(7) . . . . ? O7 C30 C33 C38 157.3(5) . . . . ? C38 C33 C34 C35 3.2(7) . . . . ? C30 C33 C34 C35 -178.3(5) . . . . ? C33 C34 C35 C36 -2.4(7) . . . . ? C33 C34 C35 C31 174.1(5) . . . . ? O10 C31 C35 C34 -144.8(5) . . . . ? O9 C31 C35 C34 31.8(7) . . . . ? O10 C31 C35 C36 31.7(7) . . . . ? O9 C31 C35 C36 -151.7(5) . . . . ? C34 C35 C36 C37 -1.4(7) . . . . ? C31 C35 C36 C37 -177.9(5) . . . . ? C35 C36 C37 C38 4.4(7) . . . . ? C35 C36 C37 C32 -171.9(5) . . . . ? O11 C32 C37 C38 -4.7(7) . . . . ? O12 C32 C37 C38 178.0(5) . . . . ? O11 C32 C37 C36 171.6(5) . . . . ? O12 C32 C37 C36 -5.7(7) . . . . ? C36 C37 C38 C33 -3.7(7) . . . . ? C32 C37 C38 C33 172.7(5) . . . . ? C34 C33 C38 C37 -0.2(7) . . . . ? C30 C33 C38 C37 -178.7(5) . . . . ? N2 C1 N1 C2 0.3(7) . . . . ? N2 C1 N1 Cd3 171.2(4) . . . . ? C3 C2 N1 C1 -0.8(8) . . . . ? C3 C2 N1 Cd3 -171.9(5) . . . . ? O1 Cd3 N1 C1 163.8(5) . . . . ? N4 Cd3 N1 C1 70.1(5) 3_565 . . . ? O9 Cd3 N1 C1 -22.5(5) . . . . ? O5 Cd3 N1 C1 -108.2(5) 2_545 . . . ? O1 Cd3 N1 C2 -27.1(5) . . . . ? N4 Cd3 N1 C2 -120.8(5) 3_565 . . . ? O9 Cd3 N1 C2 146.6(5) . . . . ? O5 Cd3 N1 C2 60.9(5) 2_545 . . . ? N1 C1 N2 C3 0.3(7) . . . . ? N1 C1 N2 C4 178.6(5) . . . . ? C2 C3 N2 C1 -0.8(8) . . . . ? C2 C3 N2 C4 -179.1(6) . . . . ? C5 C4 N2 C1 122.8(6) . . . . ? C5 C4 N2 C3 -59.3(8) . . . . ? N4 C10 N3 C8 0.2(9) . . . . ? N4 C10 N3 C7 -177.5(7) . . . . ? C9 C8 N3 C10 1.4(9) . . . . ? C9 C8 N3 C7 178.8(8) . . . . ? C6 C7 N3 C10 87.9(11) . . . . ? C6 C7 N3 C8 -89.2(11) . . . . ? N3 C10 N4 C9 -1.7(8) . . . . ? N3 C10 N4 Cd3 176.8(5) . . . 3_565 ? C8 C9 N4 C10 2.5(8) . . . . ? C8 C9 N4 Cd3 -175.7(5) . . . 3_565 ? N6 C11 N5 C12 -0.4(9) . . . . ? N6 C11 N5 Cd2 162.7(5) . . . . ? C13 C12 N5 C11 1.0(9) . . . . ? C13 C12 N5 Cd2 -164.9(5) . . . . ? O4 Cd2 N5 C11 118.6(7) 3_566 . . . ? O10 Cd2 N5 C11 -12.3(7) 4_566 . . . ? O8 Cd2 N5 C11 -108.1(7) . . . . ? O7 Cd2 N5 C11 -161.2(7) . . . . ? O4 Cd2 N5 C12 -80.4(5) 3_566 . . . ? O10 Cd2 N5 C12 148.8(5) 4_566 . . . ? O8 Cd2 N5 C12 52.9(5) . . . . ? O7 Cd2 N5 C12 -0.2(5) . . . . ? N5 C11 N6 C13 -0.3(9) . . . . ? N5 C11 N6 C14 176.5(7) . . . . ? C12 C13 N6 C11 0.9(8) . . . . ? C12 C13 N6 C14 -175.9(7) . . . . ? C15 C14 N6 C11 -116.0(9) . . . . ? C15 C14 N6 C13 60.1(10) . . . . ? N8 C20 N7 C18 -1.2(8) . . . . ? N8 C20 N7 C17 173.7(6) . . . . ? C19 C18 N7 C20 1.2(8) . . . . ? C19 C18 N7 C17 -173.6(7) . . . . ? C16 C17 N7 C20 -105.4(9) . . . . ? C16 C17 N7 C18 68.5(11) . . . . ? N7 C20 N8 C19 0.7(7) . . . . ? N7 C20 N8 Cd2 -177.7(4) . . . 4_566 ? C18 C19 N8 C20 0.1(8) . . . . ? C18 C19 N8 Cd2 178.4(5) . . . 4_566 ? O2 C21 O1 Cd3 21.7(9) . . . . ? C24 C21 O1 Cd3 -161.7(4) . . . . ? O11 Cd3 O1 C21 -79.1(5) 3_666 . . . ? N1 Cd3 O1 C21 103.3(5) . . . . ? N4 Cd3 O1 C21 -160.4(5) 3_565 . . . ? O5 Cd3 O1 C21 8.9(5) 2_545 . . . ? O1 C21 O2 Cd1 3.9(9) . . . . ? C24 C21 O2 Cd1 -172.8(3) . . . . ? O12 Cd1 O2 C21 60.4(5) 3_666 . . . ? O3 Cd1 O2 C21 154.1(5) 3_566 . . . ? O5 Cd1 O2 C21 -45.7(5) 2_545 . . . ? O6 Cd1 O2 C21 -99.8(5) 2_545 . . . ? O4 C22 O3 Cd1 -7.3(7) . . . 3_566 ? C26 C22 O3 Cd1 169.9(3) . . . 3_566 ? O3 C22 O4 Cd2 -76.8(7) . . . 3_566 ? C26 C22 O4 Cd2 106.0(5) . . . 3_566 ? O6 C23 O5 Cd3 -129.3(5) . . . 2 ? C28 C23 O5 Cd3 50.6(7) . . . 2 ? O6 C23 O5 Cd1 -2.3(5) . . . 2 ? C28 C23 O5 Cd1 177.6(4) . . . 2 ? O5 C23 O6 Cd1 2.2(5) . . . 2 ? C28 C23 O6 Cd1 -177.6(4) . . . 2 ? O8 C30 O7 Cd1 131.6(5) . . . . ? C33 C30 O7 Cd1 -49.5(8) . . . . ? O8 C30 O7 Cd2 1.4(5) . . . . ? C33 C30 O7 Cd2 -179.8(4) . . . . ? O12 Cd1 O7 C30 -17.0(6) 3_666 . . . ? O3 Cd1 O7 C30 -110.1(6) 3_566 . . . ? O5 Cd1 O7 C30 90.5(6) 2_545 . . . ? O6 Cd1 O7 C30 144.6(6) 2_545 . . . ? O12 Cd1 O7 Cd2 106.23(17) 3_666 . . . ? O3 Cd1 O7 Cd2 13.18(18) 3_566 . . . ? O5 Cd1 O7 Cd2 -146.27(16) 2_545 . . . ? O6 Cd1 O7 Cd2 -92.15(15) 2_545 . . . ? O4 Cd2 O7 C30 165.6(3) 3_566 . . . ? N8 Cd2 O7 C30 -105.6(3) 4_565 . . . ? O10 Cd2 O7 C30 -12.1(4) 4_566 . . . ? N5 Cd2 O7 C30 81.6(3) . . . . ? O8 Cd2 O7 C30 -0.8(3) . . . . ? O4 Cd2 O7 Cd1 14.88(16) 3_566 . . . ? N8 Cd2 O7 Cd1 103.75(18) 4_565 . . . ? O10 Cd2 O7 Cd1 -162.8(2) 4_566 . . . ? N5 Cd2 O7 Cd1 -69.1(2) . . . . ? O8 Cd2 O7 Cd1 -151.5(2) . . . . ? O7 C30 O8 Cd2 -1.5(6) . . . . ? C33 C30 O8 Cd2 179.6(4) . . . . ? O4 Cd2 O8 C30 -17.7(4) 3_566 . . . ? N8 Cd2 O8 C30 77.7(3) 4_565 . . . ? O10 Cd2 O8 C30 175.0(3) 4_566 . . . ? N5 Cd2 O8 C30 -100.5(3) . . . . ? O7 Cd2 O8 C30 0.8(3) . . . . ? O10 C31 O9 Cd3 -146.4(4) . . . . ? C35 C31 O9 Cd3 37.2(7) . . . . ? O11 Cd3 O9 C31 -6.4(5) 3_666 . . . ? N1 Cd3 O9 C31 172.1(5) . . . . ? N4 Cd3 O9 C31 75.2(5) 3_565 . . . ? O5 Cd3 O9 C31 -93.9(5) 2_545 . . . ? O9 C31 O10 Cd2 -30.3(6) . . . 4_565 ? C35 C31 O10 Cd2 146.2(4) . . . 4_565 ? O12 C32 O11 Cd3 19.7(13) . . . 3_666 ? C37 C32 O11 Cd3 -157.4(6) . . . 3_666 ? O11 C32 O12 Cd1 -23.0(7) . . . 3_666 ? C37 C32 O12 Cd1 154.0(3) . . . 3_666 ? C7 C6 O13 C5 -78.5(10) . . . . ? C4 C5 O13 C6 175.0(5) . . . . ? C17 C16 O14 C15 -173.0(7) . . . . ? C14 C15 O14 C16 -162.2(7) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.971 _refine_diff_density_min -1.401 _refine_diff_density_rms 0.137 #===END data_compound10 _database_code_depnum_ccdc_archive 'CCDC 665633' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H20 N4 O5 Zn' _chemical_formula_sum 'C14 H20 N4 O5 Zn' _chemical_formula_weight 389.71 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.6850(11) _cell_length_b 11.5890(12) _cell_length_c 14.1580(14) _cell_angle_alpha 90.00 _cell_angle_beta 111.857(2) _cell_angle_gamma 90.00 _cell_volume 1627.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1853 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 28.4 _exptl_crystal_description Block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.591 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 808 _exptl_absorpt_coefficient_mu 1.542 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.560 _exptl_absorpt_correction_T_max 0.742 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area-detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 9606 _diffrn_reflns_av_R_equivalents 0.0672 _diffrn_reflns_av_sigmaI/netI 0.0907 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 28.35 _reflns_number_total 3759 _reflns_number_gt 1823 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT software (Bruker, 1999)' _computing_structure_solution 'SHELXS-97(Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0800P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0085(19) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3759 _refine_ls_number_parameters 208 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1521 _refine_ls_R_factor_gt 0.0782 _refine_ls_wR_factor_ref 0.2088 _refine_ls_wR_factor_gt 0.1798 _refine_ls_goodness_of_fit_ref 1.179 _refine_ls_restrained_S_all 1.188 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.20154(8) 0.22456(6) 0.39420(5) 0.0558(3) Uani 1 1 d . . . C1 C 0.3926(8) 0.2875(6) 0.2953(6) 0.0692(19) Uani 1 1 d . . . H1 H 0.3410 0.2473 0.2369 0.083 Uiso 1 1 calc R . . C2 C 0.4663(8) 0.3534(6) 0.4485(6) 0.074(2) Uani 1 1 d . . . H2 H 0.4749 0.3688 0.5151 0.089 Uiso 1 1 calc R . . C3 C 0.5494(8) 0.3932(6) 0.4015(8) 0.082(2) Uani 1 1 d . . . H3 H 0.6255 0.4392 0.4302 0.098 Uiso 1 1 calc R . . C4 C 0.5486(10) 0.3764(8) 0.2248(7) 0.094(3) Uiso 1 1 d . . . H4A H 0.5715 0.4576 0.2271 0.113 Uiso 1 1 calc R . . H4B H 0.4797 0.3603 0.1586 0.113 Uiso 1 1 calc R . . C5 C 0.6744(9) 0.3029(7) 0.2397(8) 0.099(3) Uani 1 1 d . . . H5A H 0.7117 0.3227 0.1889 0.119 Uiso 1 1 calc R . . H5B H 0.7428 0.3164 0.3066 0.119 Uiso 1 1 calc R . . C6 C 0.7401(8) 0.1082(6) 0.2359(5) 0.072(2) Uiso 1 1 d . . . H15A H 0.7824 0.1360 0.1904 0.086 Uiso 1 1 calc R . . H15B H 0.7013 0.0333 0.2110 0.086 Uiso 1 1 calc R . . C7 C 0.8438(8) 0.0926(7) 0.3353(6) 0.082(2) Uani 1 1 d . . . H7A H 0.8838 0.1667 0.3614 0.099 Uiso 1 1 calc R . . H7B H 0.9141 0.0434 0.3295 0.099 Uiso 1 1 calc R . . C8 C 0.8237(7) -0.0669(5) 0.4505(5) 0.0554(16) Uani 1 1 d . . . H8 H 0.8830 -0.1170 0.4372 0.066 Uiso 1 1 calc R . . C9 C 0.6863(9) 0.0069(7) 0.5114(6) 0.091(3) Uani 1 1 d . . . H9 H 0.6330 0.0165 0.5499 0.109 Uiso 1 1 calc R . . C10 C 0.7015(10) 0.0849(6) 0.4460(6) 0.083(2) Uani 1 1 d . . . H10 H 0.6593 0.1564 0.4300 0.100 Uiso 1 1 calc R . . C11 C 0.1293(8) 0.3793(6) 0.5054(5) 0.0598(17) Uani 1 1 d . . . C12 C 0.0502(7) 0.4635(5) 0.5435(4) 0.0556(16) Uani 1 1 d . . . H12 H 0.1161 0.5178 0.5882 0.067 Uiso 1 1 calc R . . C13 C -0.0125(10) 0.4067(8) 0.6060(7) 0.101(3) Uiso 1 1 d . . . C14' C 0.1103(13) 0.1139(10) 0.2172(11) 0.064(3) Uiso 0.60 1 d PD . . C14 C 0.0218(17) 0.1902(13) 0.1697(10) 0.071(5) Uiso 0.40 1 d PD . . N1 N 0.3689(6) 0.2872(4) 0.3801(4) 0.0581(14) Uani 1 1 d . . . N2 N 0.4977(6) 0.3512(5) 0.3026(5) 0.0687(16) Uani 1 1 d . . . N3 N 0.7895(6) 0.0397(5) 0.4082(4) 0.0639(15) Uani 1 1 d . . . N4 N 0.7618(6) -0.0889(4) 0.5122(4) 0.0565(14) Uani 1 1 d . . . O1 O 0.0743(7) 0.3188(6) 0.4300(5) 0.0674(18) Uani 0.80 1 d P . . O2' O 0.216(3) 0.404(2) 0.471(2) 0.080(7) Uiso 0.20 1 d P . . O1' O 0.047(3) 0.297(3) 0.468(3) 0.078(9) Uiso 0.20 1 d P . . O2 O 0.2540(7) 0.3676(5) 0.5627(5) 0.0749(17) Uiso 0.80 1 d P . . O3 O 0.0528(14) 0.2898(11) 0.1789(10) 0.081(4) Uiso 0.40 1 d PD . . O3' O 0.0802(9) 0.2041(9) 0.2599(6) 0.073(2) Uani 0.60 1 d PD . . O4' O 0.2085(11) 0.0605(8) 0.2536(8) 0.087(3) Uani 0.50 1 d P . . O4 O 0.0995(13) 0.1319(12) 0.2632(9) 0.079(4) Uiso 0.50 1 d PD . . O5 O 0.6333(5) 0.1847(4) 0.2293(4) 0.0714(13) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0702(6) 0.0533(5) 0.0572(5) 0.0059(3) 0.0393(4) 0.0093(4) C1 0.074(5) 0.071(5) 0.065(5) 0.013(4) 0.029(4) -0.008(4) C2 0.072(5) 0.058(4) 0.088(6) -0.004(4) 0.026(5) 0.002(4) C3 0.062(5) 0.057(5) 0.134(8) -0.005(5) 0.046(5) 0.001(4) C5 0.088(6) 0.084(6) 0.155(9) 0.045(5) 0.081(6) 0.018(5) C7 0.082(6) 0.083(5) 0.096(6) 0.034(4) 0.050(5) -0.001(4) C8 0.062(4) 0.050(4) 0.063(4) 0.006(3) 0.033(4) 0.005(3) C9 0.143(8) 0.079(5) 0.080(5) 0.025(4) 0.076(6) 0.053(5) C10 0.130(7) 0.063(5) 0.076(5) 0.007(4) 0.061(5) 0.035(5) C11 0.073(5) 0.057(4) 0.062(4) 0.004(3) 0.039(4) 0.001(4) C12 0.064(4) 0.067(4) 0.040(3) -0.004(3) 0.024(3) 0.002(3) N1 0.073(4) 0.050(3) 0.057(3) 0.002(3) 0.031(3) -0.007(3) N2 0.069(4) 0.064(4) 0.082(4) 0.016(3) 0.039(4) 0.002(3) N3 0.075(4) 0.051(3) 0.066(3) 0.010(3) 0.026(3) -0.005(3) N4 0.071(4) 0.054(3) 0.050(3) -0.002(2) 0.029(3) 0.007(3) O1 0.092(5) 0.064(4) 0.057(4) -0.012(3) 0.041(4) 0.001(3) O3' 0.076(6) 0.085(7) 0.067(5) 0.017(5) 0.036(5) 0.030(5) O4' 0.091(8) 0.069(6) 0.074(6) -0.026(5) -0.002(6) 0.037(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O3' 1.875(8) . ? Zn1 O1 1.952(6) . ? Zn1 N4 1.999(5) 3_656 ? Zn1 N1 2.007(6) . ? Zn1 O4 2.068(14) . ? Zn1 O2' 2.32(3) . ? Zn1 O1' 2.41(3) . ? C1 N2 1.315(8) . ? C1 N1 1.316(8) . ? C1 H1 0.9300 . ? C2 N1 1.364(9) . ? C2 C3 1.374(10) . ? C2 H2 0.9300 . ? C3 N2 1.387(10) . ? C3 H3 0.9300 . ? C4 N2 1.429(10) . ? C4 C5 1.539(12) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 O5 1.429(9) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 O5 1.420(8) . ? C6 C7 1.442(10) . ? C6 H15A 0.9700 . ? C6 H15B 0.9700 . ? C7 N3 1.491(8) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 N4 1.302(7) . ? C8 N3 1.362(7) . ? C8 H8 0.9300 . ? C9 C10 1.346(10) . ? C9 N4 1.369(8) . ? C9 H9 0.9300 . ? C10 N3 1.349(9) . ? C10 H10 0.9300 . ? C11 O1 1.229(9) . ? C11 O2' 1.23(3) . ? C11 O1' 1.27(3) . ? C11 O2 1.283(9) . ? C11 C12 1.515(9) . ? C12 C13 1.451(10) . ? C12 C12 1.549(12) 3_566 ? C12 H12 0.9800 . ? C13 C14 1.401(17) 4_566 ? C13 C14' 1.649(17) 4_566 ? C14' O4 0.733(14) . ? C14' O4' 1.160(14) . ? C14' C14 1.286(14) . ? C14' O3' 1.306(15) . ? C14' C13 1.649(17) 4_565 ? C14 O3 1.195(14) . ? C14 O3' 1.206(13) . ? C14 C13 1.401(17) 4_565 ? C14 O4 1.442(15) . ? N4 Zn1 1.999(5) 3_656 ? O1 O1' 0.74(3) . ? O1 O2' 1.71(3) . ? O2' O2 1.28(3) . ? O3 O3' 1.463(15) . ? O3' O4 0.859(11) . ? O4' O4 1.476(17) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3' Zn1 O1 92.8(3) . . ? O3' Zn1 N4 117.6(4) . 3_656 ? O1 Zn1 N4 104.6(2) . 3_656 ? O3' Zn1 N1 104.5(3) . . ? O1 Zn1 N1 123.8(3) . . ? N4 Zn1 N1 112.9(2) 3_656 . ? O3' Zn1 O4 24.5(3) . . ? O1 Zn1 O4 109.7(4) . . ? N4 Zn1 O4 95.4(4) 3_656 . ? N1 Zn1 O4 106.9(4) . . ? O3' Zn1 O2' 119.1(7) . . ? O1 Zn1 O2' 46.3(7) . . ? N4 Zn1 O2' 115.6(7) 3_656 . ? N1 Zn1 O2' 79.5(7) . . ? O4 Zn1 O2' 143.5(7) . . ? O3' Zn1 O1' 98.9(8) . . ? O1 Zn1 O1' 15.4(7) . . ? N4 Zn1 O1' 89.2(7) 3_656 . ? N1 Zn1 O1' 134.1(8) . . ? O4 Zn1 O1' 110.5(9) . . ? O2' Zn1 O1' 54.7(10) . . ? N2 C1 N1 112.2(7) . . ? N2 C1 H1 123.9 . . ? N1 C1 H1 123.9 . . ? N1 C2 C3 107.7(7) . . ? N1 C2 H2 126.1 . . ? C3 C2 H2 126.1 . . ? C2 C3 N2 106.6(7) . . ? C2 C3 H3 126.7 . . ? N2 C3 H3 126.7 . . ? N2 C4 C5 110.2(7) . . ? N2 C4 H4A 109.6 . . ? C5 C4 H4A 109.6 . . ? N2 C4 H4B 109.6 . . ? C5 C4 H4B 109.6 . . ? H4A C4 H4B 108.1 . . ? O5 C5 C4 107.3(7) . . ? O5 C5 H5A 110.3 . . ? C4 C5 H5A 110.3 . . ? O5 C5 H5B 110.3 . . ? C4 C5 H5B 110.3 . . ? H5A C5 H5B 108.5 . . ? O5 C6 C7 116.7(7) . . ? O5 C6 H15A 108.1 . . ? C7 C6 H15A 108.1 . . ? O5 C6 H15B 108.1 . . ? C7 C6 H15B 108.1 . . ? H15A C6 H15B 107.3 . . ? C6 C7 N3 111.8(6) . . ? C6 C7 H7A 109.3 . . ? N3 C7 H7A 109.3 . . ? C6 C7 H7B 109.3 . . ? N3 C7 H7B 109.3 . . ? H7A C7 H7B 107.9 . . ? N4 C8 N3 110.7(5) . . ? N4 C8 H8 124.7 . . ? N3 C8 H8 124.7 . . ? C10 C9 N4 109.2(6) . . ? C10 C9 H9 125.4 . . ? N4 C9 H9 125.4 . . ? C9 C10 N3 107.0(6) . . ? C9 C10 H10 126.5 . . ? N3 C10 H10 126.5 . . ? O1 C11 O2' 88.3(13) . . ? O2' C11 O1' 121(2) . . ? O1 C11 O2 122.4(7) . . ? O2' C11 O2 61.4(13) . . ? O1' C11 O2 125.6(15) . . ? O1 C11 C12 121.8(7) . . ? O2' C11 C12 126.5(13) . . ? O1' C11 C12 103.8(16) . . ? O2 C11 C12 115.4(6) . . ? C13 C12 C11 111.7(6) . . ? C13 C12 C12 113.0(7) . 3_566 ? C11 C12 C12 112.4(6) . 3_566 ? C13 C12 H12 106.4 . . ? C11 C12 H12 106.4 . . ? C12 C12 H12 106.4 3_566 . ? C14 C13 C12 133.4(11) 4_566 . ? C14 C13 C14' 49.1(7) 4_566 4_566 ? C12 C13 C14' 105.3(8) . 4_566 ? O4 C14' O4' 100.0(18) . . ? O4 C14' C14 86.6(16) . . ? O4' C14' C14 165.0(16) . . ? O4' C14' O3' 124.0(13) . . ? C14 C14' O3' 55.4(8) . . ? O4 C14' C13 123.8(19) . 4_565 ? O4' C14' C13 127.8(12) . 4_565 ? C14 C14' C13 55.4(9) . 4_565 ? O3' C14' C13 108.2(9) . 4_565 ? O3 C14 O3' 75.1(12) . . ? O3 C14 C14' 119.1(15) . . ? O3' C14 C14' 63.1(9) . . ? O3 C14 C13 147.1(15) . 4_565 ? O3' C14 C13 134.2(12) . 4_565 ? C14' C14 C13 75.6(11) . 4_565 ? O3 C14 O4 108.1(14) . . ? C13 C14 O4 98.0(11) 4_565 . ? C1 N1 C2 106.9(6) . . ? C1 N1 Zn1 125.0(5) . . ? C2 N1 Zn1 127.2(5) . . ? C1 N2 C3 106.5(6) . . ? C1 N2 C4 127.7(7) . . ? C3 N2 C4 125.7(7) . . ? C10 N3 C8 106.8(5) . . ? C10 N3 C7 128.6(6) . . ? C8 N3 C7 124.5(6) . . ? C8 N4 C9 106.2(5) . . ? C8 N4 Zn1 125.1(4) . 3_656 ? C9 N4 Zn1 127.8(4) . 3_656 ? O1' O1 C11 76(3) . . ? O1' O1 O2' 119(3) . . ? C11 O1 O2' 45.9(9) . . ? O1' O1 Zn1 120(3) . . ? C11 O1 Zn1 113.0(6) . . ? O2' O1 Zn1 78.2(9) . . ? C11 O2' O2 61.3(13) . . ? C11 O2' O1 45.8(10) . . ? O2 O2' O1 93.5(16) . . ? C11 O2' Zn1 93.0(14) . . ? O2 O2' Zn1 97.0(14) . . ? O1 O2' Zn1 55.5(8) . . ? O1 O1' C11 70(3) . . ? C11 O1' Zn1 87.8(17) . . ? C11 O2 O2' 57.3(13) . . ? C14 O3 O3' 52.8(8) . . ? O4 O3' C14 86.9(12) . . ? C14 O3' C14' 61.4(8) . . ? O4 O3' O3 132.7(13) . . ? C14 O3' O3 52.1(8) . . ? C14' O3' O3 101.1(9) . . ? O4 O3' Zn1 90.4(11) . . ? C14 O3' Zn1 168.8(11) . . ? C14' O3' Zn1 112.0(8) . . ? O3 O3' Zn1 124.8(8) . . ? C14' O4 O3' 110.1(19) . . ? C14' O4 C14 62.9(13) . . ? O3' O4 C14 56.6(10) . . ? C14' O4 O4' 50.8(14) . . ? O3' O4 O4' 136.3(16) . . ? C14 O4 O4' 112.5(12) . . ? C14' O4 Zn1 137.7(19) . . ? O3' O4 Zn1 65.0(11) . . ? C14 O4 Zn1 120.7(11) . . ? O4' O4 Zn1 101.7(7) . . ? C6 O5 C5 112.5(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C2 C3 N2 1.2(8) . . . . ? N2 C4 C5 O5 62.8(10) . . . . ? O5 C6 C7 N3 63.1(9) . . . . ? N4 C9 C10 N3 -1.8(10) . . . . ? O1 C11 C12 C13 82.4(9) . . . . ? O2' C11 C12 C13 -163.1(17) . . . . ? O1' C11 C12 C13 50.3(17) . . . . ? O2 C11 C12 C13 -91.0(8) . . . . ? O1 C11 C12 C12 -45.9(10) . . . 3_566 ? O2' C11 C12 C12 68.6(19) . . . 3_566 ? O1' C11 C12 C12 -78.0(17) . . . 3_566 ? O2 C11 C12 C12 140.7(7) . . . 3_566 ? C11 C12 C13 C14 29.6(14) . . . 4_566 ? C12 C12 C13 C14 157.6(11) 3_566 . . 4_566 ? C11 C12 C13 C14' 77.0(8) . . . 4_566 ? C12 C12 C13 C14' -155.0(7) 3_566 . . 4_566 ? O4 C14' C14 O3 76(2) . . . . ? O4' C14' C14 O3 -41(7) . . . . ? O3' C14' C14 O3 52.2(15) . . . . ? C13 C14' C14 O3 -148(2) 4_565 . . . ? O4 C14' C14 O3' 23.7(16) . . . . ? O4' C14' C14 O3' -93(6) . . . . ? C13 C14' C14 O3' 159.6(13) 4_565 . . . ? O4 C14' C14 C13 -136.0(18) . . . 4_565 ? O4' C14' C14 C13 108(6) . . . 4_565 ? O3' C14' C14 C13 -159.6(13) . . . 4_565 ? O4' C14' C14 O4 -117(7) . . . . ? O3' C14' C14 O4 -23.7(16) . . . . ? C13 C14' C14 O4 136.0(18) 4_565 . . . ? N2 C1 N1 C2 -1.2(8) . . . . ? N2 C1 N1 Zn1 168.8(4) . . . . ? C3 C2 N1 C1 -0.1(7) . . . . ? C3 C2 N1 Zn1 -169.8(5) . . . . ? O3' Zn1 N1 C1 -13.2(6) . . . . ? O1 Zn1 N1 C1 -116.7(5) . . . . ? N4 Zn1 N1 C1 115.7(5) 3_656 . . . ? O4 Zn1 N1 C1 12.1(7) . . . . ? O2' Zn1 N1 C1 -130.8(8) . . . . ? O1' Zn1 N1 C1 -131.4(12) . . . . ? O3' Zn1 N1 C2 154.7(6) . . . . ? O1 Zn1 N1 C2 51.3(6) . . . . ? N4 Zn1 N1 C2 -76.4(6) 3_656 . . . ? O4 Zn1 N1 C2 -179.9(6) . . . . ? O2' Zn1 N1 C2 37.2(8) . . . . ? O1' Zn1 N1 C2 36.5(12) . . . . ? N1 C1 N2 C3 1.9(8) . . . . ? N1 C1 N2 C4 -176.4(7) . . . . ? C2 C3 N2 C1 -1.9(8) . . . . ? C2 C3 N2 C4 176.5(7) . . . . ? C5 C4 N2 C1 -102.9(9) . . . . ? C5 C4 N2 C3 79.0(9) . . . . ? C9 C10 N3 C8 1.3(9) . . . . ? C9 C10 N3 C7 -178.0(8) . . . . ? N4 C8 N3 C10 -0.2(8) . . . . ? N4 C8 N3 C7 179.1(6) . . . . ? C6 C7 N3 C10 -66.5(10) . . . . ? C6 C7 N3 C8 114.4(8) . . . . ? N3 C8 N4 C9 -0.9(8) . . . . ? N3 C8 N4 Zn1 -171.3(4) . . . 3_656 ? C10 C9 N4 C8 1.7(10) . . . . ? C10 C9 N4 Zn1 171.7(6) . . . 3_656 ? O2' C11 O1 O1' 161(3) . . . . ? O2 C11 O1 O1' 107(3) . . . . ? C12 C11 O1 O1' -66(3) . . . . ? O1' C11 O1 O2' -161(3) . . . . ? O2 C11 O1 O2' -54.1(13) . . . . ? C12 C11 O1 O2' 133.0(14) . . . . ? O2' C11 O1 Zn1 44.0(13) . . . . ? O1' C11 O1 Zn1 -117(3) . . . . ? O2 C11 O1 Zn1 -10.1(10) . . . . ? C12 C11 O1 Zn1 177.0(4) . . . . ? O3' Zn1 O1 O1' 114(3) . . . . ? N4 Zn1 O1 O1' -5(3) 3_656 . . . ? N1 Zn1 O1 O1' -137(3) . . . . ? O4 Zn1 O1 O1' 96(3) . . . . ? O2' Zn1 O1 O1' -117(4) . . . . ? O3' Zn1 O1 C11 -159.4(6) . . . . ? N4 Zn1 O1 C11 81.1(6) 3_656 . . . ? N1 Zn1 O1 C11 -49.9(7) . . . . ? O4 Zn1 O1 C11 -177.6(6) . . . . ? O2' Zn1 O1 C11 -30.6(10) . . . . ? O1' Zn1 O1 C11 87(3) . . . . ? O3' Zn1 O1 O2' -128.8(10) . . . . ? N4 Zn1 O1 O2' 111.7(9) 3_656 . . . ? N1 Zn1 O1 O2' -19.3(10) . . . . ? O4 Zn1 O1 O2' -147.0(10) . . . . ? O1' Zn1 O1 O2' 117(3) . . . . ? O1 C11 O2' O2 -128.9(9) . . . . ? O1' C11 O2' O2 -117(2) . . . . ? C12 C11 O2' O2 101.8(13) . . . . ? O1' C11 O2' O1 12.3(19) . . . . ? O2 C11 O2' O1 128.9(9) . . . . ? C12 C11 O2' O1 -129.3(13) . . . . ? O1 C11 O2' Zn1 -32.6(8) . . . . ? O1' C11 O2' Zn1 -20(2) . . . . ? O2 C11 O2' Zn1 96.3(11) . . . . ? C12 C11 O2' Zn1 -161.9(8) . . . . ? O1' O1 O2' C11 -21(3) . . . . ? Zn1 O1 O2' C11 -139.2(11) . . . . ? O1' O1 O2' O2 22(3) . . . . ? C11 O1 O2' O2 43.2(10) . . . . ? Zn1 O1 O2' O2 -96.1(13) . . . . ? O1' O1 O2' Zn1 118(3) . . . . ? C11 O1 O2' Zn1 139.2(11) . . . . ? O3' Zn1 O2' C11 90.9(14) . . . . ? O1 Zn1 O2' C11 28.0(9) . . . . ? N4 Zn1 O2' C11 -57.9(15) 3_656 . . . ? N1 Zn1 O2' C11 -168.3(14) . . . . ? O4 Zn1 O2' C11 87.6(17) . . . . ? O1' Zn1 O2' C11 11.1(13) . . . . ? O3' Zn1 O2' O2 152.4(11) . . . . ? O1 Zn1 O2' O2 89.5(16) . . . . ? N4 Zn1 O2' O2 3.6(17) 3_656 . . . ? N1 Zn1 O2' O2 -106.8(14) . . . . ? O4 Zn1 O2' O2 149.0(10) . . . . ? O1' Zn1 O2' O2 72.6(16) . . . . ? O3' Zn1 O2' O1 63.0(10) . . . . ? N4 Zn1 O2' O1 -85.8(8) 3_656 . . . ? N1 Zn1 O2' O1 163.7(8) . . . . ? O4 Zn1 O2' O1 59.6(15) . . . . ? O1' Zn1 O2' O1 -16.8(10) . . . . ? O2' O1 O1' C11 15(2) . . . . ? Zn1 O1 O1' C11 108.6(17) . . . . ? C11 O1 O1' Zn1 -108.6(17) . . . . ? O2' O1 O1' Zn1 -93(3) . . . . ? O2' C11 O1' O1 -22(3) . . . . ? O2 C11 O1' O1 -97(3) . . . . ? C12 C11 O1' O1 127(2) . . . . ? O1 C11 O1' Zn1 41.6(19) . . . . ? O2' C11 O1' Zn1 20(2) . . . . ? O2 C11 O1' Zn1 -55.4(18) . . . . ? C12 C11 O1' Zn1 168.6(5) . . . . ? O3' Zn1 O1' O1 -67(3) . . . . ? N4 Zn1 O1' O1 175(3) 3_656 . . . ? N1 Zn1 O1' O1 53(4) . . . . ? O4 Zn1 O1' O1 -90(3) . . . . ? O2' Zn1 O1' O1 52(3) . . . . ? O3' Zn1 O1' C11 -130.2(14) . . . . ? O1 Zn1 O1' C11 -63(3) . . . . ? N4 Zn1 O1' C11 111.9(15) 3_656 . . . ? N1 Zn1 O1' C11 -10(2) . . . . ? O4 Zn1 O1' C11 -152.6(13) . . . . ? O2' Zn1 O1' C11 -10.8(12) . . . . ? O1 C11 O2 O2' 67.2(15) . . . . ? O1' C11 O2 O2' 109(2) . . . . ? C12 C11 O2 O2' -119.4(15) . . . . ? O1 O2' O2 C11 -34.0(7) . . . . ? Zn1 O2' O2 C11 -89.6(12) . . . . ? C14' C14 O3 O3' -46.8(13) . . . . ? C13 C14 O3 O3' -157(3) 4_565 . . . ? O4 C14 O3 O3' -15.6(9) . . . . ? O3 C14 O3' O4 -154.5(16) . . . . ? C14' C14 O3' O4 -20.0(14) . . . . ? C13 C14 O3' O4 8(2) 4_565 . . . ? O3 C14 O3' C14' -134.4(15) . . . . ? C13 C14 O3' C14' 28.0(18) 4_565 . . . ? O4 C14 O3' C14' 20.0(14) . . . . ? C14' C14 O3' O3 134.4(15) . . . . ? C13 C14 O3' O3 162(3) 4_565 . . . ? O4 C14 O3' O3 154.5(16) . . . . ? O3 C14 O3' Zn1 -78(5) . . . . ? C14' C14 O3' Zn1 56(5) . . . . ? C13 C14 O3' Zn1 84(6) 4_565 . . . ? O4 C14 O3' Zn1 76(5) . . . . ? O4' C14' O3' O4 -59(2) . . . . ? C14 C14' O3' O4 140(3) . . . . ? C13 C14' O3' O4 122(3) 4_565 . . . ? O4 C14' O3' C14 -140(3) . . . . ? O4' C14' O3' C14 162(2) . . . . ? C13 C14' O3' C14 -17.5(11) 4_565 . . . ? O4 C14' O3' O3 -175(2) . . . . ? O4' C14' O3' O3 126.8(15) . . . . ? C14 C14' O3' O3 -35.1(11) . . . . ? C13 C14' O3' O3 -52.6(11) 4_565 . . . ? O4 C14' O3' Zn1 51(2) . . . . ? O4' C14' O3' Zn1 -8.1(18) . . . . ? C14 C14' O3' Zn1 -170.0(12) . . . . ? C13 C14' O3' Zn1 172.5(6) 4_565 . . . ? C14 O3 O3' O4 36(2) . . . . ? C14 O3 O3' C14' 39.7(13) . . . . ? C14 O3 O3' Zn1 166.6(13) . . . . ? O1 Zn1 O3' O4 -135.0(12) . . . . ? N4 Zn1 O3' O4 -27.0(13) 3_656 . . . ? N1 Zn1 O3' O4 99.0(12) . . . . ? O2' Zn1 O3' O4 -175.2(14) . . . . ? O1' Zn1 O3' O4 -120.8(14) . . . . ? O1 Zn1 O3' C14 149(5) . . . . ? N4 Zn1 O3' C14 -103(5) 3_656 . . . ? N1 Zn1 O3' C14 23(5) . . . . ? O4 Zn1 O3' C14 -76(5) . . . . ? O2' Zn1 O3' C14 109(5) . . . . ? O1' Zn1 O3' C14 163(5) . . . . ? O1 Zn1 O3' C14' -159.0(9) . . . . ? N4 Zn1 O3' C14' -51.0(9) 3_656 . . . ? N1 Zn1 O3' C14' 75.0(9) . . . . ? O4 Zn1 O3' C14' -24.0(11) . . . . ? O2' Zn1 O3' C14' 160.8(11) . . . . ? O1' Zn1 O3' C14' -144.8(11) . . . . ? O1 Zn1 O3' O3 78.8(9) . . . . ? N4 Zn1 O3' O3 -173.2(8) 3_656 . . . ? N1 Zn1 O3' O3 -47.2(9) . . . . ? O4 Zn1 O3' O3 -146.2(16) . . . . ? O2' Zn1 O3' O3 38.7(12) . . . . ? O1' Zn1 O3' O3 93.0(11) . . . . ? C14 C14' O4' O4 115(7) . . . . ? O3' C14' O4' O4 32.4(14) . . . . ? C13 C14' O4' O4 -148(3) 4_565 . . . ? O4' C14' O4 O3' 134.0(16) . . . . ? C14 C14' O4 O3' -32(2) . . . . ? C13 C14' O4 O3' -76(2) 4_565 . . . ? O4' C14' O4 C14 166.4(17) . . . . ? O3' C14' O4 C14 32(2) . . . . ? C13 C14' O4 C14 -43.5(14) 4_565 . . . ? C14 C14' O4 O4' -166.4(17) . . . . ? O3' C14' O4 O4' -134.0(16) . . . . ? C13 C14' O4 O4' 150(2) 4_565 . . . ? O4' C14' O4 Zn1 59(3) . . . . ? C14 C14' O4 Zn1 -107(2) . . . . ? O3' C14' O4 Zn1 -75(2) . . . . ? C13 C14' O4 Zn1 -150.4(13) 4_565 . . . ? C14 O3' O4 C14' 35(2) . . . . ? O3 O3' O4 C14' 7(3) . . . . ? Zn1 O3' O4 C14' -134(2) . . . . ? C14' O3' O4 C14 -35(2) . . . . ? O3 O3' O4 C14 -27.6(16) . . . . ? Zn1 O3' O4 C14 -169.1(11) . . . . ? C14 O3' O4 O4' 88(2) . . . . ? C14' O3' O4 O4' 54(2) . . . . ? O3 O3' O4 O4' 61(3) . . . . ? Zn1 O3' O4 O4' -80.6(19) . . . . ? C14 O3' O4 Zn1 169.1(11) . . . . ? C14' O3' O4 Zn1 134(2) . . . . ? O3 O3' O4 Zn1 141.5(17) . . . . ? O3 C14 O4 C14' -117(2) . . . . ? O3' C14 O4 C14' -143(2) . . . . ? C13 C14 O4 C14' 42.8(18) 4_565 . . . ? O3 C14 O4 O3' 26.0(16) . . . . ? C14' C14 O4 O3' 143(2) . . . . ? C13 C14 O4 O3' -174.2(17) 4_565 . . . ? O3 C14 O4 O4' -105.6(16) . . . . ? O3' C14 O4 O4' -131.6(17) . . . . ? C14' C14 O4 O4' 11.4(14) . . . . ? C13 C14 O4 O4' 54.2(15) 4_565 . . . ? O3 C14 O4 Zn1 14(2) . . . . ? O3' C14 O4 Zn1 -11.5(11) . . . . ? C14' C14 O4 Zn1 131(2) . . . . ? C13 C14 O4 Zn1 174.3(9) 4_565 . . . ? C14' O4' O4 O3' -78(2) . . . . ? C14' O4' O4 C14 -13.1(16) . . . . ? C14' O4' O4 Zn1 -144(2) . . . . ? O3' Zn1 O4 C14' 93(3) . . . . ? O1 Zn1 O4 C14' 142(2) . . . . ? N4 Zn1 O4 C14' -111(2) 3_656 . . . ? N1 Zn1 O4 C14' 5(3) . . . . ? O2' Zn1 O4 C14' 100(3) . . . . ? O1' Zn1 O4 C14' 158(3) . . . . ? O1 Zn1 O4 O3' 48.6(12) . . . . ? N4 Zn1 O4 O3' 156.2(11) 3_656 . . . ? N1 Zn1 O4 O3' -87.9(12) . . . . ? O2' Zn1 O4 O3' 7(2) . . . . ? O1' Zn1 O4 O3' 65.0(14) . . . . ? O3' Zn1 O4 C14 10.6(10) . . . . ? O1 Zn1 O4 C14 59.2(13) . . . . ? N4 Zn1 O4 C14 166.8(12) 3_656 . . . ? N1 Zn1 O4 C14 -77.4(13) . . . . ? O2' Zn1 O4 C14 18(2) . . . . ? O1' Zn1 O4 C14 75.5(15) . . . . ? O3' Zn1 O4 O4' 135.8(16) . . . . ? O1 Zn1 O4 O4' -175.6(7) . . . . ? N4 Zn1 O4 O4' -68.0(8) 3_656 . . . ? N1 Zn1 O4 O4' 47.9(8) . . . . ? O2' Zn1 O4 O4' 143.0(13) . . . . ? O1' Zn1 O4 O4' -159.2(10) . . . . ? C7 C6 O5 C5 72.6(8) . . . . ? C4 C5 O5 C6 176.7(6) . . . . ? _diffrn_measured_fraction_theta_max 0.924 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 1.620 _refine_diff_density_min -0.466 _refine_diff_density_rms 0.111 #===END